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 April 2020

The Definitive Peer-Reviewed Cosmetic Science Resource

Weighing SPF
Test Alternatives

Sun Care Mild Malodor

Myths and Claims Control

Assets of Aloe

Validating
Sunscreen Safety

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CT19_ad_template.indd 2 3/13/20 10:52 AM
GCI_full page ad.indd 1 12/20/19 9:51 AM
Cover Story Contents | C&T
April 2020 | Volume 135, number 4
®

6 Editor’s Note
Solving Sun Protection

8 Industry Insight
Sunscreen Myths, Claims and Consumer Confidence
by B. Diffey, Ph.D.

72 Ad Index

46
Market Intelligence
12 Product Roundup

16 Technology Launches

20 Expert Opinions: Sun Protection

8
Research
22 Aloe: Activity, Consistency,
Authenticity and More: A Review
by J.M. Marsh, Ph.D. and M.S.J. Simmonds

32 Evoking Emotion
Internal and External Factors
in Sensitive Skin
by K. Steventon, Ph.D.

Testing
38 Testing Tactics in Hair:

22
Conscientious Claims
Consumer Perception Before Formulation
by T.A. Evans, Ph.D.

40 Good as Gold
Validating Alternative SPF Test Methods
by U. Osterwalder, et al.

46 Standardizing Safety
ISO Validation and Sun Protection Tests
by M. Pissavini, Ph.D.

Peer-reviewed content, designated by this icon, ensures

the insights we deliver are vetted, authentic and reliable for readers.

2 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

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CT19_ad_template.indd 2 3/18/20 10:32 AM

Contents | C&T
54
52 [video] Novel In vitro
SPF Test Method Validated
with M. Pissavini, Ph.D.
Formulating
54 Mind Your Microbes
Gentle Malodor Protection
Supports the Axillary Microbiome
by F. Genrich, Ph.D, et al.
54 From the Vault: Protecting Skin
64 Formulating Forum: Eye Opener
Combined Formulation Strategy
Ensures Mascara Success
by N. Lionetti, et al.
70 Sun Care Formulary
DM29 Expanded Sun Care Formulary
Peer-reviewed content, designated by this icon, ensures
the insights we deliver are vetted, authentic and reliable for readers.
facebook.com/CandTmagazine
Cosmetics & Toiletries
4 | www.CosmeticsandToiletries.com Vol. 135, No. 1 | January 2020
CT2004_TOC_Masthead_fcx_DM.indd 4
Editor’s
9 note | C&T ®
®
ER
WINN The Definitive Peer-Reviewed Cosmetic Science Resource
EDITORIAL
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@cosmeticsandtoiletries Allured Business Media makes all attempts to publish accurate information; however, this publication may contain technical
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3/25/20 10:20 AM
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 Editor’s Note | C&T ®

Solving Sun Protection

Rachel L. Grabenhofer
Managing Editor
rgrabenhofer@allured.com

The premier peer-reviewed

resource ensuring reliable
insights to meet cosmetic
consumer demands.

Scientific
Advisory Board
Eric Abrutyn
TPC2 Advisors Ltd.

Jean-Christophe Choulot
Sun protection is a mystery, and not as easily solved as we once thought. The Caudalíe
story starts with the classic slick of ZnO down a lifeguard’s nose, which was Zoe Diana Draelos, M.D.
worn as a badge of summer honor and did a reasonably good job of physically Dermatology
Consulting Services
preventing sunburn. The industry would eventually uncover that inorganic
sunscreens mainly reflect in the UVA and absorb in the UVB range. The scene Angela R. Eppler, Ph.D.
GlaxoSmithKline
also changed when the visibly white sunscreen became esthetically undesired,
and product developers found themselves shrinking TiO2 and ZnO particles to Trefor Evans, Ph.D.
TA Evans LLC/TRI Princeton
micro and nano sizes to make them imperceptible.
Enter: organic sunscreens, e.g., octocrylene, avobenzone and octinoxate, S. Peter Foltis
Independent Consultant
whose mechanisms were different and unlocked new secrets to effectively
protect users. Taking their variety of efficacies across different wavelengths, Mindy Goldstein, Ph.D.
Mindy S. Goldstein, Ph.D. Consulting
along with those of inorganic filters, led to puzzle-piecing filters together for
greater efficacy. Eventually, though, stability issues with organics came to light, John Jiménez
Belcorp Colombia
prompting the need for photostabilizers and raising questions around their
Karl Laden, Ph.D.
potentially sensitizing effects. Inorganics, too, were investigated for stability Alpa Cosmetics
and safety issues. Indeed, the entire electromagnetic spectrum was taken into
Howard I. Maibach, M.D.
question, insofar as: which wavelengths cause what effects in the human body? University of California, San Francisco
which peripheral wavelengths, i.e., infrared and high energy visible light, are
Prithwiraj Maitra, Ph.D.
of concern? and even what alternative light sources, e.g., blue light emitting Allergan/Skinmedica
personal devices, should be assessed?
Jennifer Marsh, Ph.D.
Positive biological effects from sun exposure also were revealed and in Procter & Gamble
relation, the possible negative effects of screening out too much. Vitamin D
Marc Pissavini, Ph.D.
production, for one, became a major focus and concern. More recently, Coty-Lancaster
connections between UV and the skin microbiome are under examination.1 As
Luigi Rigano, Ph.D.
both can modulate the immune response, could one be at odds with the other? Industrial Consulting Research
This brings us to the focus of our current issue. As the sunscreen mystery
Sylvianne Schnebert, M.D.
has unfolded, identifying a consistent and accurate approach to measuring sun LVMH Recherche
protection has become, at best, a moving target. The ISO In vivo test method,
Ron Sharpe
described on Page 46, is viewed as the current gold standard. But as we have seen, Amway
change is inevitable as new evidence arises. So, despite reviews and updates to the Leslie C. Smith, Ph.D.
gold standard, alternative approaches may be worth exploring; several are explored Consultant
on Page 40. Also offered this month are Expert Opinions on current and future David C. Steinberg
sunscreens, and myths and more about sunscreens from renowned sunscreen Steinberg & Associates
researcher Brian Diffey, Ph.D., on Page 8. We hope the concepts examined here Peter Tsolis
bring you one step closer to closing the sunscreen case; at least for now. The Estée Lauder Companies

Russel Walters, Ph.D.

References Johnson & Johnson
1. https://www.frontiersin.org/articles/10.3389/
fmicb.2016.01235/full Claudie Willemin
Independent Consultant

6 | www.CosmeticsandToiletries.com Shuliang Zhang, Ph.D.

Coty, Inc.

CT2004_Editors_Note_fcx.indd 6 3/18/20 2:52 PM

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 Industry Insight | C&T ®

Sunscreen Myths, Claims and

Consumer Confidence
Sunscreens have improved immensely in the past 40 years
thanks to advances in formulation and a deeper under-
standing of sunlight and exposure. As a natural extension
of progress, however, new pain points have emerged;
these are discussed in brief in this commentary from
world-renowned sunscreen expert Brian Diffey, Ph.D., of
Newcastle University. Continue reading on Page DM1 of
the April digital magazine.

Exposure Myths
Misunderstandings about environmental sun exposure
are common in the dermatological and cosmetic literature. It
is a fact1 that both UVA and erythemal UV (largely UVB) vary
over the course of a clear day in an approximate bell-shaped
fashion beginning at sunrise, reaching a peak around noon
and ending at sunset. Yet it is not uncommon to read in
the literature phrases such as: UVB intensity declines from
noontime apex, but UVA intensity remains relatively constant
throughout the day.2
Likewise, measurements show unequivocally that UVA
and UVB both show a daily variation throughout the year
that peaks in the summer months and reaches a minimum in
mid-winter, with a summer to winter variation that becomes
more marked as we move further from the equator. For
example, in New York (latitude 40.8°N), the mid-winter and
mid-summer UV indices on a clear day are 2 and 10, respec-
tively, while the corresponding UVA ambient levels over a
winter and summer day are about 40 J/cm2 and 170 J/cm2,
respectively. Nevertheless, we find statements such as: It is
useful to remember that the level of UVA reaching the earth’s
surface is very similar in both summer and winter.3
Both of these examples from the dermatological literature
are clearly wrong, and misinformation such as this may have
contributed to the promotion of the need for year-round sun
protection even at northerly latitudes.
For example, the American Academy of Dermatology
(AAD) recommends that everyone should apply SPF 30 (or
higher) sunscreen every day before going outdoors.4 Yet esti-
mates for northern Europe5 indicate that during day-to-day
outdoor exposure, we get less than the equivalent of 1 MED
(minimal erythema dose) in skin type II on about 360 days
per year, a daily exposure of less than 0.1 MED for about six
months of the year, and less than 0.01 MED on about 30 days
per year.
So is this advice really necessary for people living in the
northern regions of Europe (e.g., UK) and North America, Brian Diffey, Ph.D.
given that some exposure to sunshine is essential for the Emeritus Professor
healthy maintenance of our vitamin D levels? Obviously, it is of Photobiology,
a different scenario during recreational exposure, when we Newcastle University

may be in strong sunshine for several hours and exposure is

8 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

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 Applications: Sun care, skin care, colour
cosmetics

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 Industry Insight | C&T ®
Figure 1. Depiction of ‘jumping ahead’
from identifying a hazard to marketing a
product with little regard for degree of
exposure or consequent health impact
much higher—sunscreens are strongly recom-
mended as part of the sun protection toolbox.
The AAD’s advice is more appropriate advice
people living in regions approaching the tropics,
since similar calculations for Florida indicate a
daily exposure of more than 0.1 MED on about
300 days per year.
IR-A Protection Claims
Laboratory studies over the past decade or so
have shown that infrared exposure can induce a
number of adverse effects both in cellular models
and in human skin,6 and these results have been
taken to infer that the infrared-A (IR-A) part of
the sun’s spectrum may contribute to premature
skin aging, necessitating the need for agents
incorporated into sunscreens that can mitigate
these effects. As a consequence, we now have
an abundance of sunscreen products claiming
to provide not only protection against UV, but
also IR-A.
What is not often appreciated, however, is
that the intensities of IR-A radiation used in
laboratory studies typically exceed greatly what
we are exposed to in sunlight. For example,
someone lying under an open cloudless sky is
only exposed to about one-tenth of the typical
IR-A intensity used in laboratory studies,7 and for
someone walking around under an open sky, the
IR-A intensity on vertical body surfaces falls to
about one-fiftieth of the typical laboratory value.
DM1 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Industry_Insight_fcx_DM.indd 10
These large differences in IR-A intensity
are important because the thermal effect of an
exposure at incident irradiances expected in
summer sunlight differs drastically from the
heating of skin when using irradiances typical of
laboratory studies. Because of the large differ-
ences in irradiance, we have to question how
relevant the findings from laboratory studies are
in the context of normal behavior and exposure
in the sun, especially since, IR-A may be more
beneficial than harmful when we are exposed to
irradiances and doses commensurate with those
in real life.8
We therefore seem to be comprising our
approach to assessing the need for IR-A protec-
tion in sunscreens by jumping directly from
identifying a possible hazard to producing and
marketing products that claim to protect against
the hazard and in the process, paying little
regard to both exposure and the consequent
harm that may, or may not, result (see Figure 1).1
Although IR-A radiation has been taken as
an example of a hazard, a similar approach
could be developed using other hazards
and consequences; for example, examining
whether sunscreens need to provide protection
against blue light, which some products are
now claiming.
Consumer Confidence
Humans need trust in the ability to rely on
others to act as they say they will, and for others
to accept we will act as we say we will.9 So, what
does it take for consumers to place their trust
and confidence in sunscreen products?
The industry must recognize the majority
of consumers simply do not understand terms
such as IR-A, broad spectrum protection or even
SPF. They place their trust in manufacturers
to take whatever steps are deemed appropriate
with regard to health and well-being, rather
than being confronted with technical choices
and claims, which many find bewildering and
unable to verify. The integrity of products and
claims, therefore, are critical if consumers are to
retain confidence in manufacturers to produce
appropriate products that allow them to enjoy
the sun safely.
A recent study10 reported that four com-
mercially available sunscreens under maximal
use conditions resulted in blood plasma con-
centrations exceeding the threshold established
by the U.S. Food and Drug Administration for
potentially waiving some non-clinical toxicol-
3/25/20 1:23 PM
 Figure 2. Trust in sunscreens under the spotlight; press headlines following the
publication of Reference 10
ogy studies for sunscreens. The press headlines
appearing after this study came out (see
Figure 2)
2 are a good example illustrating that
consumer confidence in sunscreen products is
being questioned.
While new insights into the effects of sun-
light on skin are welcomed, caution should be
exercised against assuming that just because an
adverse biological effect may be identified in the
laboratory, we must automatically try to protect
against it—even though we may not have given
proper consideration of our natural exposure
to the hazard, for example IR-A, and some
quantitative estimate of how our well-being
would suffer if we do not adopt some means
of protection.
The sunscreen industry has done much to
contribute to public health over the past 40
years. We now have products that deliver high
SPFs and balanced protection throughout the
UV. Coupled with this, products are available
in a range of formulations that provide a more
pleasurable cosmetic experience than the greasy
and oily products of many years ago.
So, in the quest for new developments, it is
vital not to compromise integrity by sacrificing
the scientific rigor of assessing the real need for
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Industry_Insight_fcx_DM.indd 11
protection against every potential hazard. Retaining
the confidence of consumers in the authenticity of
products is paramount.
References
1. Diffey, B.L. (2017). Sun Protection: A Risk Management Approach.
Bristol: IOP Publishing, Bristol, p 3-18.
2. Lowe, N.J. and Friedlander, J. (1995). Prevention of photodamage
with sun protection and sunscreens. In: Gilchrest, B.A., ed, Photo-
damage. Cambridge, MA: Blackwell Science Inc., p 202.
3. Marks, R. (1992). Sun-damaged Skin. London: Martin Dunitz Ltd., p
62.
4. American Academy of Dermatology (AAD) website. (Accessed 2020,
Feb 17). 10 Skin care secrets for healthier-looking skin. Retrieved
from https://www.aad.org/skin-care-secrets/healthier-looking-skin.
5. Diffey, B.L. (2008). A behavioral model for estimating personal expo-
sure to solar ultraviolet radiation. Photochem Photobiol 84 371–375.
6. Grether-Beck, S., Marini, A., Jaenicke, T. and Krutmann, J. (2014).
Photoprotection of human skin beyond ultraviolet radiation. Photo-
dermatol Photoimmunol Photomed 30 167-174.
7. Diffey, B. and Cadars, B. (2016). An appraisal of the need for infrared
radiation protection in sunscreens. Photochem Photobiol Sci 15
361-364.
8. Barolet, D., Christiaens, F. and Hamblin, M.R. (2016). Infrared and
skin: Friend or foe. J Photochem Photobiol B: Biology 155 78-85.
9. O’Neill, O. (2002). A Question of Trust: The BBC Reith Lectures.
Cambridge University Press, Cambridge.
10. Matta, M.K., Zusterzeel, R., … Pilli, N.R. et al. (2019). Effect of
sunscreen application under maximal use conditions on plasma
concentration of sunscreen active ingredients: A randomized clinical
trial. JAMA 321 2082-2091.
| DM2
3/25/20 1:23 PM
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 Product Roundup [Ingredients, Equipment & Services]
Highlighting innovative ingredients, services and products

Pureact SIB-10 Silube CSO Di-25

Innospec Inc.
innospecinc.com
Pureact SIB-10 (INCI: Disodium Laureth Sulfosuccinate (and)
Sodium Cocoyl lsethionate (and) Cocamidopropyl Betaine) is
a mild, sulfate-free, surfactant blend optimized to produce
foam in finished products. This rich combination gives a thick,
voluminous and stable lather, ideal for premium shampoos and
body washes. High viscosity systems are obtained with Pureact
SIB-10 by simply adding salt, alkanolamides or polymeric rheol-
ogy modifiers.
Siltech
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Silube CSO Di-25 (INCI: Pending) is a PEG-free anionic o/w emulsifier
ideal for natural oil incorporation. The product is gentle on the skin and
suitable for cold processing. Typical applications are sunscreens with
chemical filters, body lotions, face creams and color cosmetics.

Capsicum in Sweet Almond Oil

Bio-Botanica Inc.
bio-botanica.com/product/capsicum-in-sweet-
almond-oil-9825sa
Capsicum in Sweet Almond Oil
(INCI: Capsicum Frutescens
Resin (and) Prunus Amygdalus SensAmone P5
Dulcis (Sweet Almond) Oil) Mibelle Group
includes sweet almond oil, which mibellebiochemistry.com/sensamone-p5
is full of vitamin E, vitamin A,
monosaturated fatty acids, SensAmone P5 (INCI: Pentapeptide-59 (and) Hydrogenated Lecithin
protein, potassium and (and) Butyrospermum Parkii (Shea) Butter (and) Phenethyl Alcohol (and)
zinc. The fatty acids help Ethylhexylglycerin (and) Maltodextrin (and) Water (Aqua)) is an encapsu-
to retain moisture and can lated biomimetic peptide based on sea anemone venom and designed
heal chapped, irritated to inhibit the pain receptor TRPV1. In sensitive skin, TRPV1 is over-
skin. Capsicum may help reactive, which leads to itching and stinging sensations. The product
with atopic dermatitis, reduces skin sensitivity and reactivity upon irritation for a relieved and
rheumatoid arthritis more resistant skin.
and osteoarthritis.

Emulium Dolcea MB
Gattefossé
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The Emulium Dolcea MB (INCI: Cetearyl Alcohol (and) Glyceryl Stearate (and) Jojoba
Esters (and) Helianthus Annuus (Sunflower) Seed Wax (and) Sodium Stearoyl Glutamate
(and) Water (Aqua) (and) Polyglycerin-3) composition provides a great performance/sta-
bility/sensory ratio. It is compatible with natural polysaccharides, which have insufficient
stabilizing properties, and thus makes natural cosmetic formulations easier.

12 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Mrkt_Roundup_fcx.indd 12 3/18/20 11:53 AM

 Hydrosella
IFF/LucasMeyer Cosmetics
lucasmeyercosmetics.com/en/products
Hydrosella (INCI: Glycerin (and) Water (Aqua) (and)
Erythritol (and) Hibiscus Sabdariffa Fruit Extract) is
a new generation of
naturally hydrating
active ingredients
extracted from a
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Hibiscus, selected for
its high natural betaine
content. Stimulating the
production of organic
osmolytes and acting
Siddha Herbs Extract Range
on the root cause of
Campo Research Pte. Ltd. skin dryness, it reduces
campo-research.com water loss up to 72 hr
Siddha Herbs Extract Range (INCI: Varies) offers functional novelty for after application.
cosmetics and personal care products from an ancient Tamil civilization
(predating all Aryan influences) that exist in Monenjo-Doro and Harap-
pan in the Indus Valley. Derivatives of Siddha knowledge are still found
in all South & Central Asian medical systems and Chinese medicine. Rosaliss
Ashland Specialty
Ingredients
ashland.com/rosaliss
Rosaliss (INCI: Water
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Glycol (and) Rosa
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Extract) biofunctional is
a natural extract of Rosa
centifolia flower and uses
Ashland’s proprietary
and patented Plant Small RNA technology (PSR), a novel green
PGA-SHM chemistry for superior efficacy. It offers outstanding efficacy to
Bloomage Freda Biopharm USA Inc. help skin achieve flawless repair.
bloomagebioactive.com
PGA-SHM (INCI: Sodium Polyglutamate) is fermented by the probiotic
Natto bacillus. The MW of PGA-SHM is 7× larger than common PGA.
It has a better film-forming ability, offers a silky skin feeling and can
effectively promote the maturation of the cornified envelope and gen-
eration of NMF, thus enhancing the skin barrier function.

SharoSun
Acme Hardesty Company/Sharon Laboratories
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SharoSun (INCI: Not Provided) is a preservative system for
sunscreen products. Paired with SharoSense Plus 184 (INCI:
Maltol (and) Didecyldimonium Burgeon-Up
Chloride), for a natural-like
Ichimaru Pharcos
system with the ideal polar-
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Sharomix Amplify AM20 Burgeon-Up (INCI: Nasturtium Officinale Leaf/Stem Extract) is a
(INCI: Phenoxyethanol (and) product focusing on R-spondin 1 (RSPO1), which has attracted
Ethylhexylglycerin (and) attention in regenerative medicine. It upregulates RSPO1
Didecyldimonium Chloride), it secretion from dermal papilla, and elongates the hair follicle by
offers a high efficacy solution promoting transition from the telogen (resting) to anagen (growth)
with reduced levels of use. phase. In addition, RSPO1 extends each follicle’s period in the
anagen phase.

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | 13

CT2004_Mrkt_Roundup_fcx.indd 13 3/18/20 11:53 AM

 Product Roundup

Scalposine
BASF Care Creations
carecreations.basf.us
Scalposine (INCI: Glycerin
(and) Water (Aqua) (and)
Sarcosine) contains a biomi-
metic amino acid that has a
prebiotic effect to reset the
scalp’s microbial ecosystem. DermalRx Acetygen
It effectively soothes the Biocogent LLC
scalp (82% of volunteers, biocogent.com
in vitro); helps reduce flakes; DermalRx Acetygen (INCI: Water (Aqua) (and) Butylene Glycol (and)
assists in rebalancing the Agrimonia Eupatoria Extract (and) Ampelopsis Grossedentata Leaf
microbiome to fight against stress, pollution and product build-up; Extract) is a botanically derived active produced from Agrimonia
and supports the reduction of hair washes (36%). eupatoria and Ampelopsis grossedentata. It is rich in bioactive flavo-
noids including dihydromyricetin and is designed to deliver beneficial
epigenetic effects. It also enhances gene expression for broad anti-
PolluProtect inflammatory, antioxidant and anti-aging benefits. It is a great addition
Contipro a.s. to any regimen to enhance natural skin repair.
contipro.com
PolluProtect's (INCI: Sodium
Hyaluronate (and) Glucoman-
nan (and) Schizophyllan
(and) Sodium Hyaluronate
Crosspolymer) active ingre-
dients offer film-forming and
anti-inflammatory effects;
skin barrier enhancement;
reduction in ROS production
in the skin; and stimulation of
antioxidant mechanisms. The ingredient also keeps all the advan-
tages of hyaluronic acid, such as anti-wrinkle and hydration.
Filagrinol
Vevy Europe SpA
vevy.com/
Filagrinol (INCI: Pollen Extract (and) Glycine Soja (Soybean) Oil Unsa-
ponifiables (and) Olea Europaea (Olive) Oil Unsaponifiables (and) Triticum
Vulgare (Wheat) Germ Oil Unsaponifiables) is an epidermal moisturizer with
anti-oxidant and anti-lipoperoxidant activity. It modulates the production
of profilaggrin and thus filaggrin, with a key role in the final keratinization
process and an increase of the NMF. It can be used for dehydrated skin, skin
aging, sun damage, dyskeratosis, rhagades, psoriasis and diabetic skin.

Asyntra CBD-Alt
Sytheon
sytheonltd.com
Grape Seed Oil Asyntra CBD-Alt (INCI: Isosorbide Dicaprylate
Arista Industries, Inc. (and) Bakuchiol (and) Ethyl Linoleate) is a
aristaindustries.com patent-pending, crafted blend of ingredients
Grape Seed Oil (INCI: Vitis Vinifera (Grape) Seed Oil) is that acts alone or in synergy with CBD/hemp
a versatile, lightweight, noncomedogenic oil used in a oil. It maintains a level of anandamide through
variety of cosmetic and personal care applications. Rich in the modulation of the ECS, stimulating healing
vitamin E, it contains polyphenols that help to reduce signs effects as demonstrated through decreased
of premature aging and reduce inflammation. stress and increased ceramides. This results
in a stronger barrier for smoother, hydrated
and healthier skin.

14 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Mrkt_Roundup_fcx.indd 14 3/18/20 11:53 AM


  



    
 
   
 
    
 
   

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 New Ingredients & Technologies
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16 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

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 EXPERT
OPINIONS
Sun Protection
DNA Protection Factor,
Eco Concerns,
Pigment Alternatives,
User Safety and More

S
Contributors:
RACHEL L. GRABENHOFER,
COSMETICS & TOILETRIES

HOWARD EPSTEIN, PH.D.,

EMD PERFORMANCE MATERIALS
un protection is practically ubiquitous in
YOUNG BAEK KIM, P.H.D., products today; from color cosmetics and
NANO AND MICRO TECHNOLOGIES, INC.
facial creams to even hair and scalp protec-
AND PAICHAI UNIVERSITY
tion. Whether users finally understand the
CAMILLE MARTIN, SEASPIRE, INC. dangers of over-exposure, or the undesired
KEVIN O’LENICK, SURFATECH CORP. effects of premature aging have made a
bigger impact, the bottom line is there’s a surge in demand for sun
protection—to the tune of a 5.8% CAGR between 2016 and 2024,

20 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Expert_Opinions_fcx.indd 20 3/18/20 1:35 PM

 according to Transparency Market Research.1
Sun protection as a category also has expe-
rienced an evolution. Gone are the days of just
“UV protection.” Technology has empowered our
understanding of the biological effects of UV-A
versus UV-B, infrared and even high energy visible/
blue light protection. In fact, as we’ve learned, the
sources of these wavelengths are no longer limited
to the sun or even the duration of direct exposure.
For one, light emissions from our personal
devices are a new threat—which actually makes
the designation of sun protection in and of itself
a misnomer. And, new research points to the fact
that DNA damage continues even in the dark, after
direct exposure ceases.2
Add to this the fact that traditional sunscreens
incorporate skin care benefits and vice versa,
and the very idea of a stand-alone sun protection
category becomes almost obsolete, replaced by
skin care enhanced by protection against pollut-
ants, heat, cold and all the elements (including
sun). Whatever we call it, there remains a need
to protect human skin against electromagnetic
radiation—and a brief survey of the literature and
industry experts, provided here, demonstrates
some recent insights in this arena.
Visible and Infrared
Wavelengths
Singer and co-authors addressed the need to
further explore approaches to filter visible and
near-infrared wavelengths. Their paper, published
in Current Opinion in Pharmacology, underlined
the specificity of sun protection, i.e., UV protec-
tion. “…There is preliminary data that besides UV
radiation, also visible light (VIS) and near infra-
red A (IRA) radiation may have harmful effects
on skin, resulting in photoaging and even cancer
induction,” they wrote, adding that antioxidants
and DNA repair enzymes are being incorporated
into sunscreens to enhance skin protection before
and even after sun exposure. Furthermore, they
point to the need to more closely examine recent
concerns over the reported negative impact of
specific UV filters on the environment, for example,
coral bleaching.3
Howard Epstein, Ph.D., director
of technical services for EMD
Performance Materials, underlined
the industry’s interest in visible and
infrared wavelengths, too. “There
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Expert_Opinions_fcx.indd 21
is growing interest in blue light protection and to
some extent, IR-A protection as well,” he writes.
“What is interesting about blue light is this particu-
lar wavelength (500-700 nm) seems to have a more
visible impact on darker skin types.” He added that
research by his company suggests there are two
mechanisms that may explain this effect.
“One pathway is an oxidative mechanism, and
the second is a non-oxidative biological receptor
located on the surface of the melanocyte, known as
opsin-3. As we gain more understanding regard-
ing how these receptors interact with each other,
we will move closer to personalized skin care,” he
notes. Or perhaps even custom sun care?
Indeed, high-energy visible (HEV) or blue
light appears to deserve specialized attention. As
Epstein explained, his company has evaluated
European-marketed sunscreen products and found
that high SPFs, i.e., 30 and 50, actually do not
protect against blue light.
In relation, EMD tested some of its ingredients
for efficacy in this regard. “Coated inorganic filters
can mitigate HEV,” Epstein says. “We evaluated
Eusolex-TS (INCI: Titanium Dioxide (and) Alu-
mina (and) Stearic Acid), Eusolex T-PEO (INCI:
Titanium Dioxide (and) Alumina (and) Manganese
Dioxide) and Eusolex T-AVO (INCI: Titanium
Dioxide (and) Silica) [and found these] to be quite
effective. We also confirmed that skin color-correct-
ing fillers can provide HEV light mitigation, e.g.,
RonaFlair Balance Blue (INCI: Titanium Dioxide
(and) Mica (and) Tin Oxide).”
Personalized Protection
How else might sun care be personalized?
Epstein expanded, “To me, personalized skin care
means making good skin care products better skin
care products. It means accurately predicting the
most appropriate skin care regimen based on an
individual’s skin type, diet and lifestyle.”
Epstein shared his positive outlook on just
how this might be accomplished. “We have made
great advances in understanding how ingredients
work. Using an individual’s gene profile, and
with a better understanding of cell communica-
tion, we will have the ability to suggest the best
C&T Sponsored Webcast Videos
Find current and upcoming webcasts at
www.CosmeticsandToiletries.com
| 21
3/25/20 1:40 PM
 Expert Opinions: Sun Protection
ingredients to use. Opportunities will be in
new targeted antioxidants and ingredients with
light-protective properties.”
DNA Protection Factor
Josse, et al., recently proposed, in the
British Journal of Dermatology,4 a method to
determine a DNA protection factor for sun care
products. As described in the article abstract,
“Solar UV radiation is readily absorbed by
DNA and triggers the formation of dimeric
pyrimidine photoproducts such as cyclobutane
pyrimidine dimers (CPDs).” Their work (cur-
rently in production) appears to focus on the
capability of products to decrease this negative
biological effect.
Calcium Carbonate Booster
A recent patent5 assigned to Omya Inter-
national describes a functionalized calcium
carbonate to boost sun protection efficacy.
Disclosed is a composition providing UV-A and/
or UV-B protection comprising at least one
inorganic UV filter and surface-reacted calcium
carbonate. By adding this calcium carbonate,
DM3 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Expert_Opinions_irv.indd 22
the inventors claim it is possible to reduce
the amount of inorganic UV filter required to
achieve the desired SPF. They note this may
be particularly advantageous in cases where
an inorganic UV filter is nano-sized, since the
amount of nano-sized materials that may be
present in cosmetic compositions is regulated
and limited in many countries.
Bio-compatible and
Biodegradable
Organosilica Nanoparticles
Work conducted by Yoo, et al., sought to
address the safety and aesthetic limitations
of currently available sun protection materi-
als. Their paper, published in the American
Chemical Society’s (ACS’s) Applied Materials
& Interfaces,6 explains the development of,
“biocompatible and biodegradable sunscreens
by facile synthesis of organosilica nanoparticles
(o-SNPs) with self-encapsulated phenyl motifs
using phenylsilane precursors.” According
to the paper, the physical structure of these
materials is controlled such that they are large
3/18/20 11:56 AM
 enough to reflect UVA but small enough to values of particles are found in UVA regions.
go unnoticed on skin. They also are said to Safer and longer lasting sunscreens may be
generate a negligible amount of ROS upon UV formulated using these ingredients.”
exposure, and to adhere to the outer layers of
skin without penetration. Photostability, Safety and
Pigment Alternatives
Permeation Prevention Camille Martin, Chief Executive Officer for
In relation, Young Baek Kim, Ph.D., Seaspire, Inc., also points the continuing chal-
president and professor of Nano and Micro lenge to stabilize UV filters. “Studies suggest
Technologies, Inc. (N&M), and PaiChai Uni- commonly used UV filters have a causative
versity, respectively, emphasizes concerns effect on carcinogenesis and disease, due to
overs sunscreens penetrating the skin. “Many their limited photostability and their tendency
sunscreens contain skin-permeable UV filters to behave as photosensitizers,” she writes.
in concentrations higher than 20% w/w,” he However, the topical application of antioxi-
writes. “The U.S. Food and Drug Administra- dants can help to provide protection against
tion’s (FDA’s) recent report on the absorption reactive oxygen species (ROS) produced by
of filters into the bloodstream might have solar radiation. “Such antioxidants include
stirred the market a little bit. Especially in Asia, phenolics, flavonoids and carotenoids and are
many people apply sunscreens on daily basis.” currently used in many skin care products to
He added that Asian consumers are, indeed, directly eliminate or minimize the undesir-
concerned about the safety of sunscreens. “The able reactions that result from oxidation,” she
market for safer sunscreens is not [something] explains. Martin adds that sunscreen formula-
the cosmetics industry should wait for the tions should include antioxidants to enhance
development of. [It] is a market the cosmetics the photoprotective activity of actives and to
industry should develop [now] for users’ safety.” function as a secondary strategy for correcting
Furthermore, he adds that long-lasting UV-induced cellular damage.
sunscreens, free from aesthetic and safety As an alternative to traditional UV filters,
issues, are pursued and highly needed by many Martin proposes natural pigments. “Bio-derived
consumers. “With skin troubles, pregnancy, pigments great alternatives to commercially
children and [outdoor jobs exposing workers]
to the sun long periods time, if offerings are
manufactured at reasonable prices, the market
will be huge.”
What might these innovations look like?
Kim explains, “Particles and molecules with
a MW higher than 500 Daltons are known to
be skin-impermeable; [for example], silicone
ingredients [such as those developed by N&M]
including Polysilicone-24 (INCI: poly(p-
Methoxycinnamidopropylsilsesquioxane)).
These products are either skin-impermeable,
insoluble particles (70 to 130 nm), or molecules
with a MW higher than 500 Daltons.”
Furthermore, oils containing particles in
concentrations as high as 40% w/w are report-
edly spreadable and do not develop opaqueness.
“When mixed with organic filters or zinc oxide,
high in vitro SPF values are obtained. Soluble
products are very soluble in ethanol and par-
tially in propylene glycol, and form long lasting
film on the skin. Photostability is dependent on
the structure. Most interestingly, lambda max

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | DM4

CT2004_Expert_Opinions_irv.indd 23 3/18/20 11:56 AM

 Expert Opinions: Sun Protection

available UV-filters due their structural com- Trials in Testing

plexity, high molar absorptivity and enhanced
Untangling the complex interaction of light
photostability,” she writes. “Aquatic organisms
with the human biology has proven nearly
such as fish, algae, seaweed, bacteria, lichens
impossible. While the negative effects of given
and fungi have developed biological strate-
wavelengths in excessive doses to skin is
gies to counteract the harmful effects of UV
well-known, the somewhat-unknown holistic
radiation via the synthesis of UV-absorbing
implications of preventing light from reaching
metabolites. These metabolites have been dem-
the human body creates a fragile dynamic.
onstrated to provide a range of skin-protective
Drawing the lines to declare sunscreen
benefits by not only filtering UV radiation,
efficacy and safety poses a major challenge
but also [imparting] antioxidant activity
to product developers and regulators. What
that can reduce the impact of UV-induced
aspects should be measured? Are they realisti-
ROS generation.”
cally relevant? What exactly are they measuring,
Seaspire, Inc., produces such biological pig-
and how? Are they universally reproducible?
ments—Xanthochromes—which are reportedly
As new insights are revealed, iterations are
found naturally in cephalopods and arthropods.
made to existing approaches. Take the Inter-
“[These] multifunctional, sustainable materials
national Organization for Standardization’s
protect against solar radiation and can be used
(ISO’s) update7 to the existing “gold standard”
in preventative skin care, all while reducing the
In vivo SPF method, for example. In February
negative downstream effects that are inher-
2020, ISO reported several updates:
ent in current sunscreens,” Martin explained.
“Xanthochrome in its soluble form absorbs ~3× • The definition of the minimal erythema
more UV radiation than the common chemical response (MED) criteria was revised;
filters oxybenzone and avobenzone, at the same • The choice of eligible test subjects is now
concentrations,” she added, also noting that based solely on individual typology angle
since they occur naturally as dermal pigments (ITA°), with a requirement for the average
in arthropods and mollusks, they are inherently ITA° for the test panel to be within the
biocompatible and pose a low risk for breaking range 41° to 55°, and with a minimum
down into toxic byproducts when activated of three subjects within two of the three
by sunlight. ITA° ranges;
• The ITA° is used to define the range of
unprotected MED doses for the provi-
sional or the test day unprotected MED
determination (if no provisional MEDu
determination is made);
• Three new reference standard sunscreens
have been validated and added to the
method to validate SPF test panels for
products with SPF equal to 25 or higher
(P5, P6 and P8);
• New test methods are provided to deter-
mine the uniformity of the beam of both
large and small beam size solar simulators.
In relation, a requirement for unifor-
mity greater than or equal to 90% has
been added;
• Sunscreen application procedures have
been described in greater detail;
• Annex F was added with photographic
examples of erythema responses and
guidelines for grading; and

DM5 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Expert_Opinions_irv.indd 24 3/18/20 11:56 AM

 • Reporting tables in Annex G and the
requirements in Clause 11 have modified to
provide more complete information on the
results of the testing.
This raises more questions than answers,
and the literature is heavy with research explor-
ing new approaches to measure sun protection
efficacy. In fact, for this reason, we have dedi-
cated two main features in our current issue to
this very subject (see Pages 40 and 46).
FDA Delay, Eco Concerns
and Poised for Change
What additional concerns and trends are
shaping the sun protection market? Epstein
points to the status of the FDA’s Final Mono-
graph. “[There are concerns over] the FDA Final
Monograph. Until we know the status of organic
filters, many formulators are working on
titanium and zinc- based sun filters,” he writes.
“The challenge is to achieve high-SPF, broad-
spectrum claims with elegant aesthetics. Not to
mention [the need to address] concerns for ‘reef
friendly’ ingredients.”
Kevin O’Lenick, president of SurfaTech
Corp., agrees on the safety front, especially
when it comes to the environment. “The current
trend in sun protection is safety,” he writes.
“The consumer is more and more concerned
with their safety and the safety of the environ-
ment. They need to know these products will
protect them from harmful rays from the
sun, and that they will not have a negative
impact on the environment when they are
inevitability released.”
O’Lenick added he thinks the market is
poised for the next step. “I believe that this
market is going to change rapidly. The FDA is in
the process of evaluating active ingredients for
skin penetration, and specific actives have been
banned because of the potential harm they may
be causing to the coral reef. The consumer has
also become aware of the problem that plastics
are causing in our oceans and lakes…[and] will
demand that plastics be taken out of our sun
care products to ensure that they are not being
left in our waters.”
So, what will it take to address all of these
concerns? O’Lenick responded, “This market
demands new ingredients… New actives must
be discovered that will protect the consumer
but will also not disturb the environment.
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Expert_Opinions_irv.indd 25
We also have a need for non-plastic, water-
resistant agents to protect the consumer and
the environment.”
References
1. Transparency Market Research. (2018, Dec 17). Sun care
market is expected to reach US$24.9 billion by 2024; Grow-
ing awareness of personal care to boost global market,
says TMR. https://www.prnewswire.com/news-releases/
sun-care-market-is-expected-to-reach-us-24-9-billion-
by-2024-growing-awareness-of-personal-care-to-boost-
global-market-says-tmr-882935452.html
2. Grabenhofer, R. (2019, Dec 10). Acetyl zingerone
prevents dark CPD formation in skin. https://www.
cosmeticsandtoiletries.com/research/universitydata/
Acetyl-Zingerone-Prevents-Dark-CPD-Formation-in-
Skin-566051761.html
3. Singer, S., Karrer, S. and Berneberg, M. (2019, Jun).
Modern sun protection. Current Opinion in Pharmacology,
46 24-28. https://doi.org/10.1016/j.coph.2018.12.006
4. Josse, G., Gravier, E. and Douki, T. (2020, Feb 6). Method
for the accurate determination of the DNA protection factor
of sun care products. Brit J Derm. https://doi.org/10.1111/
bjd.18936
5. US20190380927A1 (2019, Dec 19). Functionalized calcium
carbonate for sun protection boosting. Assigned to Omya.
https://patents.google.com/patent/US20190380927A1/en
6. Yoo, J., Kim, H., Chang, H., Park, W., Hahn, S.K. and
Kwon, W. (2020, Feb 5). Biocompatible organosilica
nanoparticles with self-encapsulated phenyl motifs for
effective UV protection. ACS Appl Mater Interfaces, 12,
8, 9062-9069. https://pubs.acs.org/doi/abs/10.1021/
acsami.9b21990
7. ISO. (2019, Dec). ISO 24444:2019. Cosmetics—Sun
protection test methods—In vivo determination of the
sun protection factor (SPF). https://www.iso.org/stan-
dard/72250.html
| DM6
3/18/20 11:56 AM
Alo
Research | C&T ®

KEY POINTS
• Aloe vera has mutiple claimed skin care
benefits that link to the plant's growth,
cultivation and harvest.

• The present article explores how

sources of Aloe vera can vary in
chemistry, and what to consider when
formulating with this ingredient.

Aloe Activity, Consistency, Authenticity and More: A Review

A s the use of botanicals

in beauty continues to
increase, this article
delves deeply into what is
probably the most famous
and ubiquitous botani-
cal—Aloe vera, often called the “wonder” plant due to
its multiple claimed benefits. Despite its long history
of use, there is still debate about its composition and
how this links to measured benefits. Without doubt,
it is a fascinating plant and its utility in beauty only
looks to be growing.
As such, the present article reviews its known
benefits and how they are linked to the plant’s
growth, cultivation and harvest. It also explores how
sources of Aloe vera can vary in their chemistry, and
what to consider when formulating this ingredient in
different products.

Taxonomy and History

Officially Aloe vera (L.) Burm. f. but commonly
referred to as Aloe barbadensis Miller, the plant
is part of the genus Aloe, which contains more
than 500 different aloe species. It also belongs to

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Reproduction in English or any other language of

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© 2020 Allured Business Media.

CT2003_Testing_Marsh_irv.indd 22 3/18/20 12:13 PM

oe
Peer-reviewed

Jennifer M. Marsh, Ph.D.

The Procter & Gamble Company, Cincinnati
Monique S. J. Simmonds
Royal Botanic Gardens, Kew, Surrey, UL

Reproduction in English or any other language of all or part of this article is strictly prohibited. © 2020 Allured Business Media. Cosmetics & Toiletries® | 23

CT2003_Testing_Marsh_fcx.indd 23 3/23/20 10:02 AM

 Aloe
Today, the world demand for aloe is more
than 100 million liters and the world market
is worth more than US $600 million.
the family Asphodelaceae, which is related to
the Liliaceae family that includes garlic, onion
and asparagus. Recent genetic research of the
plant has shown it originates from the Arabian
Peninsula1 but is grown commercially in many
countries including India, South Africa, the
United States, Mexico, Venezuela and Haiti.
Aloe is a succulent with the ability to store
water in its leaves and thus is capable of grow-
ing well in arid and semi-tropical countries.
Even though it is a succulent, the plant is not
a cactus and ideally it needs > 100 cm of water
each year to grow. This availability of water has
a significant impact on the final extract’s quality.
The plant grows to a height of 60-100 cm in
its mature state, which occurs after 4-6 years,
and it can survive longer than 15 years. The
leaves can be harvested every 6-8 weeks by
removing 3-4 leaves from each plant. The active
components are found in the leaves, which
house three major structural components: the
clear inner gel, called mucilage tissue or pulp,
which is a soft slippery tissue composed of
~98% water; the middle latex, a bitter yellow
sap; and the outer thick cuticle or rind of
the leaf.
The plant’s name, aloe, means “shining bitter
substance” in Arabic, and vera means “true” in
Latin. This underlines the importance of aloe
leaves for traditional medicinal and cosmetic
use, which has been known for centuries. Well-
In North America, the Aloe vera market
reached a value of US $56.6 million in 2019,
and is expected to reach $78.9 million
by 2025.
Source: Imarc Group
24 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2003_Testing_Marsh_irv.indd 24
known and documented in the 16th century
BC, aloe is mentioned in the Egyptian Ebers
Papyrus medical record. It is also described in
the works of Dioscorides, who was an Ancient
Greek botanist and physicist living in Imperial
Rome under Emperor Nero.
In the first century AD, Nero produced a
book, the Codex Aniciae Juliane, on medicinal
herbs with illustrations of more than 600 plants
believed to have healing properties. In the illus-
tration of Aloe vera, Nero recommended using
the plant to aid and possibly heal skin ailments
and hemorrhoids. It was also well-known to the
ancient Egyptians as the “plant of mortality”
and used by notorious queens such as Nefertiti
and Cleopatra as part of their beauty regimens.
In old texts from Arabia and the Orient, aloe,
referred to as Ghrit Kumari, is an ingredient in
many recipes for digestive health.
Until the 17th century, the only official
aloe was grown on the island of Socotra in the
Indian Ocean, but as its popularity grew, so did
its reach. As it became a cost-effective crop,
new habitats were identified and from this, the
variety of product types including gels, powders,
etc., grew.
Aloe Today
Today, the world demand for aloe is more
than 100 million liters and the world market is
worth more than US $600 million. This demand
is steadily growing, with a predicted compound
annual growth rate of 7.6% between 2019 and
2024.2 Aloe is the only species not covered by the
Convention on International Trade in Endan-
gered Species (CITES) of Wild Flora and Fauna,
which places restrictions on the trade of endan-
gered plants. The issue with aloe is the pressure
of taking land from other activities, such as
food production, to meet the increasing global
demands. It is predicted there will be increasing
pressure to ensure good agronomy and harvest-
ing practices to maintain the extract’s quality.
3/18/20 12:13 PM
 Benefits of Aloe
Part of the popularity of aloe is its wide and
varied range of claimed benefits, including anti-
inflammation, laxative, anti-viral, anti-tumor,
antibacterial and antifungal benefits. Detailed
clinical studies are limited but research is avail-
able that entails these benefits, as well as studies
attempting to link its activity to specific respon-
sible components in aloe. From these studies,
more than 200 biologically active compounds in
the aloe leaf have been identified; this is per-
haps the secret to its wide-ranging efficacy and
long history.
Such findings have spawned a huge number
of different aloe products including pills, sprays,
ointments, lotions, liquids, drinks and creams
in major industries such as food and beverages,
pharmaceutical and cosmetics. In fact, nearly
40% of the global aloe market is in the cosmet-
ics space. Skin care products
make up the highest percent-
age of this, ~60%, whereas
hair and soap/bath products
each make up ~20%. These
products are either formula-
tions with added aloe or aloe
gel itself, which is often used
for moisturization or hydra-
tion in both skin and hair.
Active Constituents
Extensive research has been carried out to
identify the diversity of components in Aloe
vera; Table 1 details several, along with their
properties.3 As mentioned, the gel is ~98%
water but of the dry solids, 53% are polysaccha-
rides, 17% sugars, 16% minerals, 7% proteins
and 5% lipids. The most important constituents
of aloe gel are polysaccharides as these are
known to have anti-microbial, anti-viral and
antioxidant properties.
One specific polysaccharide of interest
is acemannan, which is a β-(1,4)-acetylated
soluble polymannose found mostly primarily
in the gel (see Figure 1).4 Its concentration in
the plant is closely linked to planting condi-
tions, and particularly to water and light levels.
Acemannan itself has been reported to have
many pharmacological and biological applica-

Figure 1. Acemannan

Table 1. Constituents identified in Aloe vera

Active Class Active Component Properties

Polysaccharides Mannose-6-phosphate
Humectancy, antimicrobial, anti-viral
and sugars Glucomannans
Aloin, emodin, barbaloin, aloetic Laxatives, analgesics, antibacterials,
Anthraquinones
acid, resistannol anti-virals
Vitamins Vitamins A, C, E, B1, B2, B6 and B12 Vitamins A, C and E are antioxidants
Catalase, cellulose, bradykinase, Bradykinase helps reduce skin
Enzymes
lipase inflammation when applied topically
Calcium, chromium, copper,
Minerals selenium, magnesium, manganese, Essential for some enzyme function
potassium, sodium, zinc
Salicylic acid has anti-inflammatory
Organic acids Sorbate, salicylic acid, uric acid
and antibacterial properties
Saponins Cleansing and antiseptic properties

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | 25

CT2003_Testing_Marsh_irv.indd 25 3/18/20 12:13 PM

 Aloe
Photos courtesy of the authors
tions in medical and industrial fields, such as
for oral diseases, cardiovascular diseases and
tumor diseases. It has been shown to promote
the formation and of dentin in teeth,5 and to
promote the mineralization of human dental
pulp.6 In addition, the data suggests a role
in healing mouth ulcers,7 and in vitro testing
shows a role in skin wound healing.8
Many studies show structural characteristics
of plant polysaccharides such as molecular
weight, chemical composition, branching
structure and conformation affect biological
activity but there are only limited studies on
acemannan. For example, it has been shown
that acetyl groups are important to the confor-
mation and physical/biological properties of the
polysaccharide. It is also known that agronomy
and processing conditions can impact this via
deacetylation but a detailed structure-activity
relationship has not been fully elucidated.
The most important actives in the latex and
rind are the anthraquinones, including aloin
(see Figure 2). These actives are documented as
laxatives and can act as analgesics, anti-bacte-
rial agents and anti-virals. Aloin was banned by
26 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2003_Testing_Marsh_irv.indd 26
Figure 2. Aloin
the U.S. Food and Drug Administration (FDA)
in 2002, however, since it may cause abdominal
spasms and pain with long-term use, and exces-
sive dosing can lead to hepatitis. The EU allows
aloin with a maximum use level in food and
beverages of at 0.1 mg/kg except for alcoholic
beverages, where the limit is 50 mg/kg. Aloin
is now mainly removed from aloe extracts,
especially for dermatologic and cosmetic uses,
as are other anthraquinones such as emodin.
In some cases, ingredients responsible
for aloe’s activity have been identified as the
polysaccharides, aloin, etc., but in other cases
there is evidence of more complex interactions
among components. Studies that research these
complex synergies are very limited. Since aloe
compositions can vary considerably, accord-
ing to agronomy and processing, this makes
scientific work more difficult; the result can
differ vastly due to the proportions of specific
actives in the extract.
There also are many reports of aloe’s efficacy
but the number of well-controlled clinical
studies is limited. In 1999, a review of the
literature was performed to identify and review
these studies.9 Only 10 were performed using
Aloe vera mono-preparations. Two trials studied
wound healing with Aloe vera and both trials
exemplified a clear result. The first as a half-face
clinical on patients that had undergone dermal
abrasion of the face due to Acne vulgaris.10
Here, wounds saturated with aloe were found to
heal 72 hours faster than control sites. A second
trial examined the rate of wound healing for
in 40 women after gynecologic surgery. Heal-
ing required an average 83 days in the control
versus 53 days for wounds treated with aloe.11
Another trial for the treatment of psoriasis
studied 60 men and women in a double-blind,
placebo-controlled manner.12 The number of
3/18/20 12:13 PM
 There is evidence that aloe gel can act as a
humectant and emollient to soften and smooth
skin and improve skin barrier function.
patients “cured,” as defined by the index of
skin lesions, was 83% for those treated with
aloe vs just 7% for the control. Positive results
also have been observed in studies of patients
with hyperlipidemia and a negative response
to diet,13 and patients with a first genital
herpes episode.14 However, no benefit was
observed in studies assessing the prevention of
radiation-induced skin injury in women with
breast cancer,15 or in studies of patients with
diabetes mellitus.16
In relation to cosmetics and personal care,
hair and skin studies are limited. There is
evidence that aloe gel can act as a humectant,
likely driven by the polysaccharide content,
and an emollient to soften and smooth skin and
improve skin barrier function.
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2003_Testing_Marsh_irv.indd 27
Extract Consistency
and Quality
One of the challenges posed by the large
demand for aloe is consistency of the extract
composition and, in turn, the potential for
variability in bioactivity. The first factor that
will influence the composition is agronomy,
including the supply of water, availability of
nitrogen and acidity of the soil. The anthraqui-
none content of aloe is closely related to water
content but also plant growth, which can vary
with rainfall or irrigation conditions.
Growing conditions: The optimum
agronomy is still not fully understood but
the preferred conditions are approximately
> 200 cm rainfall per annum, nitrogen levels of
0.4-0.5% and well-drained soil with a pH of 7.4.
| 27
3/18/20 12:13 PM
 Aloe
Clearly, areas where severe frosts can occur
should be avoided for planting, as this can
kill a crop. With these optimum conditions,
densities of up to 6,000 plants/acre can be
successfully harvested.
Harvest conditions: Another factor is the
time taken between harvesting and processing.
The aloe gel will oxidize when exposed to air,
altering sugar and polysaccharide content,
which can influence the efficacy of the gel. The
ideal time between harvesting and processing
is two to four hours, and significant loss in
biological activity has been measured after
24 hr.17 Therefore, to optimize quality, plant
processing must be located close to fields and
a good organization of harvesting and process-
ing operations is essential. The third factor
is how the plant is processed, particularly in
relation to the temperature during extraction,
as exposure to extended temperatures above
60°C can destroy the gel polysaccharides.
Adulteration concerns: A further problem
facing the aloe buyer is the adulteration of
extracts. The cost of Aloe vera raw materials is
relatively high. As such, aloe juice is sometimes
alternatively sourced—although it has been
28 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2003_Testing_Marsh_irv.indd 28
known to be adulterated with maltodextrin to
supplement or replace polysaccharides. Also,
adulteration with glucose, glycerin and malic
acid has been reported.
In fact, in 1981, the International Aloe
Science Council (IASC) was established as a
trade group for the aloe industry. It was around
this time when significant issues emerged with
inaccurate representations of the actual amount
of Aloe vera in aloe products. The group created
a certification program that allows growers,
processors and manufacturers to submit their
facilities and products to a series of tests and
audits that, upon approval, permit the use of
the IASC seal on products and literature. The
IASC website contains a list of certified compa-
nies18 offering accurate information and testing
for aloe.
Aloe analysis and authentication: Several
methods are required to determine the com-
position of aloe and the potential presence of
contaminants. A study in 2005 investigated nine
different aloe products from different suppliers
and utilized these techniques to authenticate
extract quality.19
1
HNMR, for example, was used to identify
3/18/20 12:13 PM
 the presence of polysaccharide acemannan, glucose
and malic acid, which are three major components of
aloe. Acemannan is a β-(1→4) linked mannan partially
acetylated in positions 2, 3 or 6, and this provides a
very characteristic signal that can be considered the
fingerprint of aloe. The same technique can identify
maltodextrin as a potential adulterant.
In the same study,19 free sugars were assessed by
high performance anion exchange chromatography
with pulsed amperometric detection (HPAE-PAD).
Organic acids lactic and succinic acid were also
analyzed by HPLC-UV for indicators of bacterial
fermentation and enzymatic degradation, i.e., indica-
tors of product freshness. HPLC-UV also was used as
a method to verify the absence of hydroxyanthracene
derivatives, i.e., (aloin and aloin-related compounds).
Thus, with these analytical tools, the variations in
extract quality can be shown. For this study, only three
of the nine products contained satisfactory levels of
acemannan; one showed abnormally high levels of
glucose; and one was contaminated with high levels
of aloin.

Aloe Processing
There are three basics steps to processing of aloe.17
First, the leaves are scrubbed in a bactericide since
control of bacterial proliferation is key post-harvest.
The rind is removed to yield the gel fillet. This may
be carried out manually but can be costly and time-
consuming; it may also be automated. As the highest
level of aloin is found in the rind, good quality filleting
leads to the lowest levels in the final gel. Recently,
an alternative to filleting has also been introduced
that is a cheaper and more efficient, especially for
small leaves: grinding of the whole leaf. The grind-
ing method contains activated charcoal to remove
anthraquinones, then cellulase is added to dissolve the
cellulose. The cellulosic pulp is then removed.
The second step is to kill bacteria that can break
down sugars and other plant properties. Most aloe
is pasteurized by heating it to 65°C for 15 min. It is
important to maintain a balance between the heat
needed to kill bacteria, increases to polysaccharide
molecular weight by deacetylation, and losses of
galactose-rich side chains. Recall, as stated above, that
exposure to extended temperatures above 60°C can
destroy the gel polysaccharides.
The final stage is the addition of preservatives such
as sodium benzoate, potassium sorbate, citric acid or
vitamin E. The aloe gel is typically concentrated via
a thin film evaporation and maintained at 35-45°C,
where a concentrate throughput of ~200 L/hr can
be achieved. Several factors must be controlled at

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CT2003_Testing_Marsh_irv.indd 29 3/18/20 12:13 PM

 Aloe
this stage. Exogenous contamination of cel-
lulose, for example, can cause polysaccharide
destruction and darkening can occur due to
polyphenolic group condensation.
Most resulting aloe concentrates will be sold
to the beverage industry but for cosmetic uses,
dry products are preferred for ease of transport
and storage and improved product stability over
time. In some cases, the powder will be recon-
stituted into a gel. As the desire for product
certifications increases, more products are
available as certified organic, as well as kosher
and halal.
In fact, aloe leaf juice is often used to
support organic product claims. In the United
States, for example, a product can be labeled
"organic” if it is made with more than 70%
organic ingredients. By replacing a percentage
of water in the formula with certified organic
and/or COSMOS-approved Aloe barbadensis leaf
juice, this claim can be made on the packaging.
Conclusion
Aloe vera is truly a “wonder plant.” Although
well-controlled scientific studies of its effects
are limited there is still a significant body of
evidence supporting its bioactivity in a wide
range of areas. However, it is important for for-
mulators to understand that extracts can vary
in quality according to growing conditions and
processing controls with each harvest. Certifica-
tion of quality can be carried out via the IASC
but additional authentication may be needed to
ensure the product delivers the desired benefit.
References
1. Grace, O.M., ... Buerki, S., et al. (2015). Evolutionary history
and leaf succulence as explanations for medicinal use in
aloes and the global popularity of Aloe vera. BMC Evolution-
ary Biology 15 29.
2. Unknown. (2019, May). Aloe vera extract market size and
share: Share and trends analysis report by application
(food, pharmaceutical, cosmetic), by distribution channel
(offline, online), by product (gels, capsule, powder, liquid),
and segment forecasts, 2019–2025. Grand View Research.
Retrieved from https://www.grandviewresearch.com/
industry-analysis/aloe-vera-extracts-market.
3. Lanka, S. (2018). A review on Aloe vera–The wonder
medicinal plant. J Drug Deliv Thera 8 94-99.
4. Li, C., Cui, Y., Fuwei, P., Yuliang, C., Yahui, G. and Quin, H.
(2019). Extraction, purification, structural characteristics,
biological activities and pharmacological applications of
acemannan, a polysaccharide. In Aloe vera: A Review.
Molecules 24 1554.
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CT2003_Testing_Marsh_irv.indd 30
5. Songsiripradubboob, S., Banlunara, W., Sangvanich, P.,
Trairatvorakul, C. and Thunyakitpisal, P. (2016). Clincal,
radiographic and histologic analysis of the effects of
acemannan used in direct pulp capping of human primary
teeth; Short-term outcomes. Odontology 104 329-337.
6. Jittapiromsak, N., Sahawat, D., Banlunara, W.,
Sangvanich, P. and Thunyakitpisal, P. (2010). Acemannan,
an extracted product from Aloe vera, stimulaes dental pulp
proliferation, differentiation, mineralization and dentin forma-
tion. Tissue Eng Part A 16 1997-2006.
7. Plemmons, J.M., Rees, T.D., Binnie, W.H., Wright, J.M.,
Guo, I. and Hall, J.E. (1994). Evaluation of acemannan in the
treatment of aphthous stomatitis. Wounds 6 40-45.
8. Xing, W., Guo, W., ... Zou, C.H., et al. (2015). Acemannan
accelerates cell proliferation and skin wound healing through
AKT/mTOR signaling pathway. J Dermatol Sci 79 101-109.
9. Vogler, B.K. and Ernst, E. (1999). Aloe vera: A systematic
review of its clinical effectiveness. Brit J Gen Pract 49
823-828.
10. Fulton, J.E. (1990). The stimulation of postdermabrasion
wound healing with stabilized Aloe vera gel-polyethylene
oxide dressing. J Dermatol Surg Oncl 16 460-467.
11. Schmidt, J.M. and Greenspoon, J.S. (1991). Aloe vera der-
mal wound gel is associated with a delay in wound healing.
Obstet Gynecol 1 115-117.
12. Syed, T.A., Ahmad, S.A. and Holt, A.H. (1996). Manage-
ment of psoriasis with Aloe vera extract in a hydrophilic
cream: A placebo-controlled, double-blind study. Trop Med
Int Health 1(4) 505-509.
13. Nassiff, H.A., Fajardo, F. and Velez, F. (1993). Effecto del
aloe sorbre la hyperlipidemia en pacientes refractarios a la
dieta. Rev Cuba Med Gen Integr 9 43-51.
14. Syed, T.A., Cheema, K.M., Ashaf, A. and Holt, A.H. (1996).
Aloe vera extract 0.5% in a hydrophilic cream versus Aloe
vera for the management of genital herpes in males. A
placebo-controlled double-blind, comparative study. J Eur
Acid Dermatol Venereol 7 294-295.
15. Williams, M.S., Burk, M. and Loprinzi, C.L. (1996). Phase III
double-blind evaluation of an Aloe vera gel as a prophylactic
agent for radiation-induced skin toxicity. Int J Radiat Oncol
Biol Phys 35 345-349.
16. Yongchaiyudha, S., Rungpitarangsi, V., Bunyapraphat-
sara, N., and Chokechaijareonporn, O. (1996). Antidiabetic
activity of Aloe vera L. juice. 1. Clinical trial in new cases of
diabeties mellitus. Phytomedicine 3 43-51.
17. Waller, T.A., Pelley, R.P. and Strickland, F.M. (2004).
Industrial processing and quality control of Aloe barbadensis
(Aloe vera) gel. In: Reynolds, T., ed., Aloes, The Genus Aloe.
CRC Press LLC, Boca Raton, Fl.
18. The International Aloe Science Council (IASC) website.
(Accessed 2020, Feb 5). Retrieved from https://www.iasc.
org/Home.aspx.
19. Bozzi, A., Perrin, C., Auston, S. and Arca Vera, F. (2007).
Quality and authenticity of commercial Aloe vera gel pow-
ders. Food Chem 103 22-30.
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 Research | C&T ®

KEY POINTS
• Self-esteem and first impressions have
inspired an increased demand for sensitive
skin products.

• The science behind sensitive skin is

subjective but consumers have a self-
percieved notion on sensitivity.

Evoking Emotion:
Internal and
External Factors
in Sensitive Skin
Katerina Steventon, Ph.D.
FaceWorkshops LLC
York, UK

A bout 50% of women declare they have sensitive

skin. This skin sensitivity can create emotional
turmoil when itching, burning and irritation are
not even visible, or when irregular blemishes
occur. Sensitive skin remains a largely unanswered
problem since it does not correspond to a specific
physiological pattern. It also presents the challenge of uneven skin appear-
ance ranging from dryness to oiliness. The following highlights recent work
related to sensitive skin and first impressions, interpretations in the brain,
different types of sensitivity and more.

Reproduction in English or any other language of

32 | www.CosmeticsandToiletries.com all or part of this article is strictly prohibited. Vol. 135, No. 4 | April 2020
© 2020 Allured Business Media.

CT2004_Research_Steventon_irv.indd 32 3/18/20 1:14 PM

 The negative effect of blemished
skin can create the impression
that a person is immature and
less trustworthy.

First Impressions
Judgments of character can be based on facial appearance which, in
turn, guides personal interactions in terms of social engagement and/or
avoidance. In fact, research has shown that people are particularly sensitive
to skin blemishes as these may indicate poor health and the presence of
an infectious disease. The negative effect of blemished skin also can create
the impression that a person is immature and less trustworthy—versus
the positive effects of smooth skin, which impart opposite assumptions of
trustworthiness, competency, attractiveness and health.1
This legacy of skin sensitivity, in line with unpleasant sensory symp-
toms, motivates those with sensitive skin to take skin care seriously.
Consider atopic dermatitis (AD) and allergic diseases, for example, which
have increased dramatically during the past few decades. Scientific under-
standings of the risk factors for developing these conditions and effective
preventive measures remain limited. In fact, there is evidence that skin
barrier impairment and early-life atopic dermatitis could play a causal role
in the development of skin sensitization. As such, skin care plays an impor-
tant role, and the regular use of prophylactic emollients can significantly
decrease the expression of AD while treatment continues.2

Subjective Sensations in the Brain

Skin sensitivity is also a subjective matter, as functional magnetic reso-
nance imaging (fmRI) has shown. In one study, a brain scan was performed
in attempt to objectify a neural basis for sensitive skin in subjects that had
self-perceived sensitive and non-sensitive skin. The research showed that
skin discomfort due to irritation by a lactic acid test caused increased activ-
ity in specific areas of the brain in all participants; specifically, the primary
sensorimotor cortex contralateral to the application site; and the bilateral
frontoparietal network including the parietal cortex, prefrontal areas
around the superior frontal sulcus, and the supplementary motor area.
However, the activity was significantly larger in the sensitive skin
group. Only in this group did the activity spread to other parts of the brain;
specifically, the ipsilateral primary sensorimotor cortex and the bilateral

A 2014 survey by Galderma and the National Rosacea

Society found that individuals with clear skin were more
likely than those with rosacea to be seen as relaxed
(77% vs. 64%) or charismatic (75% vs. 63%).

Source: Businesswire

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | 33

CT2004_Research_Steventon_irv.indd 33 3/18/20 1:14 PM

 Evoking Emotion
peri-insular secondary somatosensory area.
Therefore, self-perceived sensitive skin seems
to show brain activation during irritation and a
specific neurophysiological pattern.3
In dermatology, itch has been mapped in
the brain since it is a common sensory experi-
ence associated with skin inflammation. The
communitive signals between keratinocytes,
the immune system and sensory nerves are
responsible for the pathophysiology of itching.
These signals begin in the skin, proceeding to
the spinal cord and eventually ascending to the
brain, where itch is processed.4
One study comparing electroencephalog-
raphy (EEG) changes in the brain for burn
patients with chronic itch showed decreased
alpha activity in the occipital channels and
decreased low beta activity in the frontal area
under eyes-closed conditions. Itching in burns
therefore seems to be associated with brain
reorganizational changes at the cortical level, as
characterized by the EEG pattern.5
Detecting Sensitivity Across
Skin Types
The demand for cosmetics aimed at sensitive
skin is increasing; however, no arbitrary meth-
ods have been set to detect skin sensitivity. An
impaired barrier function is understood to play
one role in sensitive skin. Heightened neural
and vascular reactions are also implicated.
The lactic acid stinging test, baseline blood
flow, current perception threshold (CPT) and
capsaicin test of the nasolabial fold are stan-
dard methods often used in attempt to test for
34 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Research_Steventon_irv.indd 34
sensitive skin. Higher lactic acid response and
lower baseline CPT values are for people who
experience the sensation of stinging, burning and
itching. Interestingly, a genetic variation of the
transient receptor potential vanilloid subfamily
member 1 (TRPV1) receptor has been identified,
and unpleasant sensations demonstrate that
TRPV1 is important in the pathogenesis of sensi-
tive skin.6, 7
Notably, skin sensitivity can arise in both
dry and oily skin types. In relation, non-invasive
facial skin mapping of physiological param-
eters has come a long way; from single point
bio-instrumental evaluations, to continuous visu-
alization of skin hydration, barrier function, skin
surface pH and sebum—in all different ethnic
skin types. Dry skin, for example, can be associ-
ated with skin sensitivity and itch, and although
there is still a paucity of data for the underlying
cellular and biochemical problems in dry skin, it
is the best-mapped type so far.
In 2014, the continuous facial analysis of bio-
instrumental evaluations was developed using
a heat map approach. These maps enabled the
visualization of facial features and revealed an
unexpected complexity of facial skin, demonstrat-
ing that remarkable gradients of skin hydration,
trans-epidermal water loss (TEWL), skin surface
pH and sebum exist within short distances across
the face.
A new statistical approach is therefore
required to prove these differences in facial skin
parameters, visualize treatment efficacy and
advance a comprehensive understanding of dif-
ferences in skin physiology and related product
3/18/20 1:14 PM
 application.8 Such research underpins the con-
cept of “Corneocare,” developed by DSM, which
includes ingredients and concepts that take a
holistic approach to epidermis-related skin sen-
sations. According to the company, “combined
with appearance, [these innovations] provide
a complete beauty experience and a liberating
feeling of skin comfort with skin that is smooth
and pleasant to touch.”
Similar to dry skin mapping, facial maps
for oily skin are still missing for skin sensitivity
research. Excessive oil can lead to emotional
discomfort due to concerns such as shine,
enlarged pores, acne and a damaged skin bar-
rier. The range of skin oiliness and texture also
must be assessed by correlating instrumental
analysis with clinical scoring, as distinct areas
of the face differ in oiliness, and the quantity
and appearance of pores and comedones.
Higher clinical scores for shine intensity
and oiliness—and tendency for pigmentation—
coincide with higher objective values of sebum
production, TEWL and skin texture roughness.
Different skin characteristics also influence
the prevalence of sensitivity and blemishes in
different areas of the face.9, 10
The assessment of sensitive skin may be
influenced by factors including climate and
seasons, facial areas, phototype and lifestyle
Judgments of character can be based on facial appearance which, in turn, guides personal interactions in terms of social
engagement and/or avoidance.
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Research_Steventon_irv.indd 35
as well. For example, in terms of a lactic acid
stinging test, sensitivity differences arise between
the seasons with scores increased in the autumn.
Interestingly, in skin phototypes III and IV, the
frequency of sleep and ingestion of spicy food can
also affect skin sensitivity.11
And, as the industry has become well-aware,
skin microbiota can aggravate sensitivity. In
relation, some studies12 have suggested a rural
environment may provide protection mediated via
exposure to environmental microbes needed to
support normal immune tolerance. The triangle
of interactions between environmental microbes,
host microbiota and the immune system remains
poorly understood but likely can affect skin
sensitivity as well.
Conclusion
The challenge for the industry is to better
understand and map the interplay of factors
in different skin types and the complexities of
modern living. Formulating with a focus on the
brain’s response to skin care application, sensory
irritation inhibitors and anti-inflammatory actives
can reduce the heightened neural and vascular
response of sensitive skin, which is essential
to future skin care research and formulating.
Translating research findings early could lead to
innovative, multifactorial and targeted products
| 35
3/18/20 1:14 PM
 Evoking Emotion

to alleviate consumer symptoms and enhance their

emotional well-being.

References
1. Jaeger, B., Wagemans, F. M. A., Evans, A. M. and van Beest, I. (2018,
Jun). Effects of facial skin smoothness and blemishes on trait impres-
sions. Perception 47(6) 608-625. Available at https://www.ncbi.nlm.nih.
gov/pubmed/29580151.
2. Lowe, A. J., et al. (2018, Feb). The skin as a target for prevention of the
atopic march. Ann Allergy Asthma Immunol 120(2) 145-151. Available
at https://www.ncbi.nlm.nih.gov/pubmed/29413338.
3. Querleux, B., et al. (2008, Nov). Neural basis of sensitive skin: an fMRI
study. Skin Res Technol 14(4) 454-461. Available at https://www.ncbi.
nlm.nih.gov/pubmed/18937781.
4. Yosipovitch, G., Rosen, J. D. and Hashimoto, T. (2018, Nov). Itch:
From mechanism to (novel) therapeutic approaches. J Allergy Clin
Immunol 142(5) 1375-1390. Available at https://www.ncbi.nlm.nih.gov/
pubmed/30409247.
5. Miraval, F. K., et al. (2017, Aug). A preliminary study on qEEG in burn
patients with chronic pruritus. Ann Rehabil Med 41(4) 693-700. Avail-
able at https://www.ncbi.nlm.nih.gov/pubmed/28971055.
6. Sun, L., et al. (2016, Aug). The evaluation of neural and vascular hyper-
reactivity for sensitive skin. Skin Res Technol 41(3) 381-387. Available at
https://www.ncbi.nlm.nih.gov/pubmed/26841957.
7. Ham, H., et al. (2016, Feb). Itching sensation and neuronal sensitivity
of the skin. Skin Res Technol 22(1) 104-107. Available at https://www.
ncbi.nlm.nih.gov/pubmed/26250122.
8. Voegeli, R., Gierschendorf, J., Summers, B. and Rawlings, A. V.
(2019, Oct). Facial skin mapping: from single point bio-instrumental
evaluation to continuous visualization of skin hydration, barrier func-
tion, skin surface pH, and sebum in different ethnic skin types. Int J
Cosmet Sci 41(5) 411-424. Available at https://www.ncbi.nlm.nih.gov/
pubmed/31325176.
9. Maia Campos, P. M. B. G., Melo, M. O. and Mercurio, D. G. (2019,
Mar 26). Use of advanced imaging techniques for the characterization
of oily skin. Front Physiol. Available at https://www.ncbi.nlm.nih.gov/
pubmed/30971936.
10. Mercurio, D. G., Segura, J. H., Demets, M. B. A. and Maia Campos, P.
M. B. G. (2013, Apr). Clinical scoring and instrumental analysis to evalu-
ate skin types. Clin Exp Dermatol 38(3) 302-308. Available at https://
www.ncbi.nlm.nih.gov/pubmed/23517362.
11. Ye, C. X., et al. (2019, Sep 9). Skin sensitivity evaluation: What could
impact the assessment results? J Cosmet Dermatol. Available at
https://www.ncbi.nlm.nih.gov/pubmed/31498557.
12. Kasahara, K. (2018, Dec 7). Farm to face: environmental bacte-
ria boost skin's barrier. Cosm & Toil 8. Available at https://www.
cosmeticsandtoiletries.com/research/biology/video-Freshly-Farmed-
Bacteria-Boost-Skins-Barrier-502161681.html.

36 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Research_Steventon_irv.indd 36 3/18/20 1:14 PM

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 Testing | C&T ®

KEY POINTS
• The hair care industry is constantly
changing, as are its product claims—the
latest of which are reviewed here in the
context of science vs. consumer language.
• The author proposes first fully developing
claims that address consumer perception
to simplify formulating and ensure
products pass acceptance tests.

Testing Tactics in Hair

Conscientious
Claims Consumer Perception Before Formulation

Trefor Evans, Ph.D.

TRI Princeton, Princeton, NJ

38 | www.CosmeticsandToiletries.com
T he hair care industry has changed more over the past
decade than any other. This is not a consequence of
new technological advancements, but instead relates
to the increasingly rich, new Information Age. The
rise of the internet has been accompanied by now
commonplace phenomena such as online sales and
marketing, social media, webinars, blogging, influencers and so forth that
have forever altered the world in which we operate.

Reproduction in English or any other language of

all or part of this article is strictly prohibited.
© 2020 Allured Business Media.
Vol. 135, No. 4 | April 2020

CT2003_Testing_Evans_fcx2.indd 38 3/20/20 3:12 PM

 Advertising claims represent the
fundamental reason to believe in a product.
Perhaps most notably, smaller companies
and start-ups no longer need to battle estab-
lished incumbents for shelf space at traditional
retailers. Products can be sold via online stores
with no such space restrictions and directly
ordered from snappy, attention-grabbing
websites. Social media can be a powerful new
source for marketing and advertising and
subsequently, it becomes possible to success-
fully build brands in a manner that is different
from the past.
Yet this Information Age can similarly cause
headaches, wherein the hair care consumer can
find it difficult to process and translate the vast
quantities of information (and misinformation)
that exists in the cyber world. Accordingly,
some strange ideas can take hold and even grow
within the environment.
But this new world does not rewrite the
rules when it comes to ethically and legally
communicating product benefits to consum-
ers. These new outlets do not preclude such
smaller companies from abiding by the rules,
and all companies must ensure that commu-
nication messages and advertising claims are
effectively authenticated.
A Reason to Believe
Advertising claims represent the fundamen-
tal reason to believe in a product. In the hair
care world, these messages generally revolve
around promises of performance benefits—for
example, an improvement in sensory (softness,
smoothness) properties, manageability and/
or appearance. Further popular practice is to
communicate a magnitude of such benefits,
wherein it is commonplace to see such claims
as 10× stronger, 5× smoother, 3× shinier, etc.
Past articles in this column have described
the ways by which such measurements are
typically performed.1-3
There generally are not particularly sizable
differences in the compositions of various hair
care products on the market. By means of illus-
tration, most commercial conditioners consist
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2003_Testing_Evans_fcx2.indd 39
primarily of water, a quaternary amine surfac-
tant and a fatty alcohol co-surfactant. There
may be differences in the exact nature of these
ingredients and their levels but the fundamental
science is the same.
Accordingly, product differentiation is often
attained or attempted through aesthetics, i.e.,
an attractive fragrance, packaging, etc., and/or
an appealing communication message. There
is always the temptation to make these stories
increasingly elaborate and exorbitant to attract
consumers, but failure to deliver on these
promises can create ire in consumer, competi-
tors and others.
Previously, the product development world
was mostly self-policed by the larger compa-
nies who would challenge each other if it was
felt that any of these messages became too
egregious. Since then, consolidation within
the industry has reduced the number of big
companies, and this process does not appear so
prevalent. At the same time, consumer advo-
cacy and advertising standards groups provide
a means for consumers to air their grievances
if they feel they have been wronged by the
product claims.
C&T Webcasts
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Shampoo holds the largest market share in the
hair care segment and is estimated to grow to
US $30 billion by 2023.
Source: Schwartz Natural Cosmetics
| 39
3/25/20 11:25 AM
 Conscientious Claims
A third means of claims scrutiny becom-
ing increasingly frequent is a practice I term
cosmetic ambulance chasing. Initially, this con-
stituted lawyers attempting to find individuals
who have had (or claim to have had) an adverse
reaction to a product. But this concept has
further evolved into situations where a product
was purchased based on the claims and these
benefits were not realized by consumers, and so
a class lawsuit is filed against the company for
misleading the public.
There are now more media outlet sources
than ever before with everyone seeking content.
The trolling of advertising standard websites
represents a cheap and easy way to find subject
matter and invariably such decisions will be
sensationalized to some extent in print. This
negative publicity can irrevocably decimate
a product or brand’s legitimacy, as soon as
overnight, by questioning the fundamental
reasons for believing. Thus, before going to
market, there is a need to ensure that all claims
are airtight.
Devil in the Detail
Case in point, in 2011, a major hair care
brand was challenged via the Advertising Stan-
dards Authority (ASA) in the UK for a claim
DM7 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2003_Testing_Evans_fcx2.indd 40
that its conditioner product “made hair 10×
stronger.” In support of this claim, the company
provided the ASA with data from a repeated
grooming experiment, an approach that has
been described in past articles of this column.1
The ASA accepted the data and concluded,
“the method used by the advertiser to examine
hair strength was a consumer-relevant method
of establishing hair strength when brushing
or combing;”4 but at the same time, the ASA
questioned why testing had been performed on
chemically damaged hair.
This is a common practice in the hair
care industry, as it frequently leads to greater
A mistake commonly
encountered when
working in the claims
area is the wrong
order of operations.
3/20/20 3:13 PM
 method sensitivity,5 and it is justified by
industry folklore that most women utilize at
least one chemical treatment on their hair.
The ASA acknowledged this positioning but
asked for data to back up this stance—but this
information was not available. The company
thus received a mild slap on the wrist and was
asked to adjust its advertising to reflect that
not everyone might expect benefits of the same
magnitude. Nonetheless, headlines in the next
day’s newspapers reported how the ASA had
banned the company’s hair care ads as they
were misleading to the customer.
Because of this situation, it is necessary
to have data to back up every aspect of the
claim including method validation/justifica-
tion, hair type, application procedure, etc. It is
also prudent to ensure that all data is within
the company and at hand. When working
with companies on their claim substantiation
packages, a somewhat common occurrence is
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2003_Testing_Evans_fcx2.indd 41
to hear that critical data relates to a specific
ingredient with that information being provided
by the ingredient supplier. While not necessarily
questioning this data, it is extremely trusting
for any company to place its brand or product’s
reputation in the hands of third-party data.
Consumer or
Instrumental Data
There are two common approaches for
claims substantiation. On the one hand,
products can be given to consumer test panels,
wherein answers from questionnaires are sup-
portive of intended positions. For example, if a
majority agrees with a question that asks: “Did
this product moisturize your hair?” then the
proposition would seem justified.
A second option involves the use of instru-
mental measurements to demonstrate how the
technical properties of hair have been altered.
For example, one can measure reduced comb-
| DM8
3/20/20 3:13 PM
 Conscientious Claims
Body Talk:
Defining Volume
Click to Page 48 in the
June 2018 digital magazine.
ing forces as a result of applying a conditioner to
hair,6 or an improvement in technical shine as a
result of using a silicone-based shine serum.3
Importantly, companies are not restricted to
just one of these approaches. In fact, companies
should be regularly performing both types
of testing.
Moisture or Moisturization?
A recurring theme over the history of this
column has been the differences between “con-
sumer” language and “scientific” language.7 By
means of illustration, the author’s firm receives
regular requests to scientifically test hair treated
with a given product in attempt to demonstrate
increased water content and therefore justify a
“moisturizing” proposition. Extensive experience
with this measurement, however, has shown this
outcome never transpires.8
Yet, in consumer testing, conditioner prod-
ucts are overwhelmingly perceived to induce
some sort of “moisturization.” Therefore, such
products are changing the properties of hair
in some manner by which the consumer per-
ceives “moisturization,” although this does not
constitute an actual technical increase in hair
water content.
By far, the most pronounced technical benefit
of conditioners is an ability to substantially
lubricate the hair surface in an aesthetically
pleasing manner but “lubrication” is not a con-
sumer word. Instead, this benefit is viewed by
consumers as softness, smoothness, improved
manageability, etc. These interpretations are
largely intuitive, but others may be less literal.
For example, if a consumer senses their hair
to be damaged but the symptoms are allevi-
ated by product treatment, then the product
may be described as “repairing” the hair. The
complex physical structure of hair cannot be
technically repaired by soap and water, but the
masking of negative feel attributes equates to
this interpretation.
In a similar vein, it appears logical to
conclude that the consumer perception of hair
DM9 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2003_Testing_Evans_fcx2.indd 42
feeling “dry” equates to roughness associated
with degradation of the outer cuticle structure.9
To this end, mitigation of this occurrence is
seen as “moisturizing.”
Strength or Anti-breakage?
Another frequent request is the measure-
ment of the mechanical properties of hair
fibers10 treated with various daily-use products
to show if “strengthening” has occurred in
hair. This also scientifically never happens, but
consumer testing demonstrates a pronounced
belief that conditioner-treated hair is stronger.
An answer to this conundrum is provided by
the aforementioned repeated grooming experi-
ments, wherein treatment with traditional
conditioner products results in a dramatic
reduction in hair breakage. Past articles have
described the theory by which reduced groom-
ing forces result in lower snagging, tangling
and fatiguing forces, and accordingly lead to
less breakage.1, 11 Readers will see how surface
lubrication provided by conditioner treatments
is responsible for this possibly non-instinctive
consumer response.
'The Cart Before the Horse'
(Formula Before Claims)
A mistake commonly encountered when
working in the claims area is the wrong order of
operations; i,e., "We have a good formula, now
what claims should we make?" If the desired
claims can be identified first, then the formula
can be optimized and the likelihood of attain-
ing impressive quantitative claims is greatly
enhanced. To illustrate this point, following
is an example from the author's past product
development work.
A prototype hair gel formula was created
and demonstrated parity with the market leader
during consumer testing. Also, the formula
cost was lower than what had been stipulated
in the brief—so everyone was happy. However,
just prior to launch, marketing sought to add
an anti-humidity claim. This proposition was
not in the original brief, and so a rather basic
styling polymer had been used that exhibited
poor humidity resistance (this being the reason
for the low formula cost). Had this claim been
discussed up front, the formula could have
included a more sophisticated styling polymer
to achieve the end goal, even though it would
have cost more.
3/20/20 3:13 PM
 Conclusion
The Holy Grails of the hair industry are
extremely well entrenched but “consumer”
language is often not the same as “scientific”
language. As previously stated, the consumer
term moisturization does not equate technically
to hair water content, while what consumers
call strengthening does not equate to scientifi-
cally assessed mechanical properties.
These important findings become appar-
ent only when performing both consumer
and scientific testing. While this dual evalu-
ation adds cost to the testing process, it can
nonetheless save time of misdirected product
development work. Armed with this new infor-
mation, vastly different formulation strategies
would be employed. Moreover, this informa-
tion is pivotal in crafting convincing claims
substantiation strategies.
It is suggested, therefore, that a sensible
claims substantiation strategy should involve
utilizing instrumental testing to demonstrate
that a prototype formula or product changes
some technical property of the hair to a
meaningful extent. Then, subsequent consumer
testing reveals how these changes in fiber
properties are perceived by end users.
The need for irrevocably corroborating prod-
uct claims cannot be understated. Without such
evidence, the marketing of products becomes
analogous to snake oil salesmanship, wherein a
free-for-all of evermore outlandish propositions
ensues. In short, the legitimacy of the industry
is at stake. Ideally, this process should be self-
policed whereby companies with self-interest
will call out offenders. However, the Internet
Age has spawned so many cosmetic companies
that smaller fish can slip through the nets.
Further policing should be provided by
consumer advocacy and advertising standard
groups—even the lawyers are getting involved.
To this end, wrongdoers should, at the very
least, be on a finite timeline and ferreted
out, eventually.
Acknowledgements: This article is a variation of a
presentation given by the author at the Society of Cosmetic
Chemists 73rd Annual Scientific and Technology Showcase
in New York on Dec. 17, 2019.
References
1. Evans, T.A. (2013, Dec). Measuring hair strength, part 2:
Fiber breakage. Cosm & Toil 128(12) 854-859. Retrieved
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2003_Testing_Evans_fcx2.indd 43
from https://www.cosmeticsandtoiletries.com/testing/
efficacyclaims/premiumMeasuring-Hair-Strength-Part-II-
Fiber-Breakage-232884161.html.
2. Evans, T.A. (2019, Nov/Dec). A soft touch. Concepts
in hair softness. Cosm & Toil 134(10) 46-53. Retrieved
from https://www.cosmeticsandtoiletries.com/testing/
efficacyclaims/A-Soft-TouchConcepts-in-Hair-Soft-
ness-564871682.html.
3. Evans, T.A. (2016, Jan/Feb). Equating the measurement of
hair shine. Cosm & Toil 131(1) 28-34. Retrieved from https://
www.cosmeticsandtoiletries.com/testing/efficacyclaims/
Coiffed-Conundrum-Equating-the-Measurement-of-Hair-
Shine-367691731.html.
4. The Rose Sheet Report. (2011, Jul).
5. Evans, T.A. (2014, Nov). Hair as a test substrate in the
laboratory. Cosm & Toil. Retrieved from http://www.
cosmeticsandtoiletries.com/testing/efficacyclaims/Hair-as-
a-Test-Substrate-premium-282462371.html.
6. Evans, T.A. (2011, Aug). Evaluating hair conditioning
with instrumental combing. Cosm & Toil (126)8 558-563.
Retrieved from https://www.cosmeticsandtoiletries.com/
testing/sensory/premium-Evaluating-Hair-Conditioning-with-
Instrumental-Combing-217611571.html.
7. Evans, T.A. (2013, May). Consumer vs. scientific language:
Relating in vivo to in vitro. Cosm & Toil 128(5) 300-304.
Retrieved from https://www.cosmeticsandtoiletries.com/
testing/invitro/premium-Testing-Tactics-Consumer-vs-
Scientific-Language-Relating-In-vivo-to-In-vitro-218744901.
html.
8. Evans, T.A. (2014, Mar). Measuring the water content of
hair. Cosm & Toil 129(2) 64-69. Retrieved from https://www.
cosmeticsandtoiletries.com/testing/invitro/Measuring-the-
Water-Content-of-Hairpremium-246571251.html.
9. Evans, T.A. (2017, Apr). How damaged is your hair? Part
1: Surface damage. Cosm & Toil 132(4). 38-48. Retrieved
from https://www.cosmeticsandtoiletries.com/testing/
sensory/How-Damaged-is-Hair-Part-One-Surface-Dam-
age-417064423.html.
10. Evans, T.A. (2013, Mar). Measuring hair strength, part 1:
Stress-strain curves. Cosm & Toil 128(8) 590-594.
11. Evans, T.A. (2017, Sep). New ideas and thoughts on hair
breakage. Cosm & Toil 132(8) 46-53. Retrieved from https://
www.cosmeticsandtoiletries.com/testing/efficacyclaims/
premium-Measuring-Hair-Strength-Part-I-Stress-Strain-
Curves-218888981.html.
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| DM10
3/20/20 3:13 PM
 Testing | C&T ®

KEY POINTS
• This article presents alternative sunscreen
test methods to the gold standard ISO
24444:2019. Options range from in vivo
calibrated in silico tools and in vitro plate
procedures, to a hybrid method.

• This discussion highlights their potential

and procedures for their validation with
the aim of replacing the current standard.

Peer-reviewed

facebook.com/CandTmagazine Cosmetics & Toiletries @cosmeticsandtoiletries

Reproduction in English or any other language of

40 | www.CosmeticsandToiletries.com all or part of this article is strictly prohibited. Vol. 135, No. 4 | April 2020
© 2020 Allured Business Media.

CT2004_Testing_Osterwalder_fcx.indd 40 3/23/20 10:04 AM

 GOOD AS

GOLD Validating Alternative

SPF Test Methods
Uli Osterwalder
Sun Protection Facilitator (SPF) GmbH, Basel, Switzerland

Steffen Uhlig, Ph.D., and Bertrand Colson

QuoData Quality and Statistics GmbH

T
Berlin and Dresden (respectively), Germany

Jürgen Vollhardt, Ph.D.

DSM Nutritional Products Ltd., Basel, Switzerland

wo years ago, the current Human skin and the processes that
authors published the article, occur during sunscreen application are also
“SPF Assessment Revis- complex4, 5 and difficult to match by alterna-
ited—Status and Outlook.”1 tive templates or procedures. Therefore,
The present article provides it has taken quite some time to develop
an update on progress methods that could, for the vast variety of
toward alternative SPF methods. It also proposes a sunscreens made globally, consistently deliver
validation process for such methods with the goal of comparable results.
equivalating them to and revising the gold standard Furthermore, the In vivo SPF procedure
ISO 24444:2019.2, 3 First, however, consider the utilizes UV radiation and represents a burden
challenge of finding alternative SPF methods. to the test subjects. Therefore, alternative
The SPF In vivo test as described in the norm ISO procedures should avoid this burden. Also, the
24444 is a relatively complex method and requires very nature of human subjects intrinsically
significant equipment and time to be executed. How- causes some variation in results. The desire is
ever, because human skin serves as the template therefore to identify alternative methods with
and performance indicator, it directly connects with less variation that are more robust and agree
the application of sunscreens and potential biologi- well with in vivo SPF results.
cal damage to skin caused by UV.

Vol. 135, No.

Reproduction 4 | April
in English 2020
or any other
language of all or part of this article is strictly prohibited. © 2020 Allured Business Media. Cosmetics & Toiletries® | 41

CT2004_Testing_Osterwalder_irv.indd 41 3/18/20 1:51 PM

 Good as Gold
Complex processes occur during
sunscreen application, so it has taken some
time to develop test methods that deliver
consistent and comparable results.
Finding an alternative method that dem-
onstrates high precision is relatively easy, but
the challenge has been to find a method that
can also predict the true SPF value correctly.
This puzzle is depicted in Figure 1. Alternative
methods must also demonstrate sufficiently
good agreement with the current In vivo SPF
method. This raises several questions: How
can the agreement of two methods be tested?
How many test institutes should be involved?
How many different products and types must
be tested? And how does the method validation
differ from the routine procedure? To gain per-
Figure 1. Depiction of "roughly right" versus
"precisely wrong"
Globally, sun care products are projected to
rise at a modest CAGR of 2.15% between
2020 and 2025, with the Middle East and
Africa as the fastest-growing markets.
Source: Mordor Intelligence
42 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Testing_Osterwalder_irv.indd 42
spective, it would help to revisit ISO 24444:2010
and its recent revision, ISO 24444:2019, before
turning to alternative methods.
SPF In vivo Test
ISO 24444:2019
SPF determination began more than 50 years
ago as an outdoor method, using erythema as
the biological endpoint. UV-induced damage
triggers an inflammation reaction that creates
visible erythema via a multistep biological path-
way. The measured SPF values were very low at
that time, often just SPF 2, 3, 4, etc. Today, in
vivo SPF determination is more complex, with
protocols using standardized solar-simulated
light sources2, 3 and much higher SPF values:
SPF 30 and 50 are the most popular categories.
ISO 24444 and the very similar US-FDA 20116
are currently considered the gold standards in
sunscreen assessment, and Garzarella, et al.,
showed that both methods—ISO’s and the U.S.
Food and Drug Administration’s (FDA’s), yield
similar SPF values.7
For both protocols, the standard reference
samples P2 and P3 are examples of known
true SPF values. Data recently collected by
Alejandria, et al., for reference sample P2
shows,8 impressively, how the random/overall
error of the SPF determination can be reduced
by increasing the number of repetitions (see
Table 1). The standard error (precision) is
reduced by the square root of the number of
repetitions. On the other hand, the mean (true)
value does not change much beyond a reason-
able minimum number of repetitions.
In the case of the SPF measurement, it
is assumed that the average value from 10
volunteers is sufficient to determine the SPF
in a particular laboratory setting and routine
operation. In fact, the differences between
the standard SPF values and the average of
approximately one thousand measurements of
P2 are only 3% (ISO) and 6% (FDA), respec-
3/18/20 1:51 PM
 Table 1. Overall Determined SPF Error as a Function of Repetition

Standard, n = 1 Average of n = Repetition 

SPF of P2 Value Std. error Value Std. error (calc*) n=
ISO 24444:2010 16.1 2.42 15.6 0.1 (0.1) 1551
FDA-FM, 2011 16.3 3.43 15.4 0.12 (0.1) 952

* calc = standard error of method, divided by square root of n

tively. So, both can be considered as close to the SPF 50+, which means SPF > 60 in Europe. The
true value. new standards P5, P6 and P8 also will be used in
On the other hand, a single SPF determina- future norms of alternative SPF methods.
tion in just one laboratory can, of course, be
much further away from the true value. Miksa, Currently Available
et al., showed it is advisable to take the average Alternative SPF Methods
of at least three or four such SPF values from
The development of alternative SPF and
different test institutes, with five volunteers
UVA-PF methods has been under way for several
each, to generate a more reliable SPF value,
decades. The fact that none of these has replaced
closer to the true value,9 as can be expected
the gold standard so far shows this is not an
from statistical considerations.
easy task. Figure 2 gives an overview of SPF
assessment methods, which can be classified
Revisions3 to according to several criteria. Classical divisions
ISO 24444:2019 are along the type of method, i.e., in vivo, in vitro
The revision of ISO 24444:2019 was prepared and in silico; and the burden of UV radiation to
by Technical Committee ISO/TC 217, Cosmetics, which skin is exposed. As can be seen, and as is
over the last 3-4 years. This second edition can- explained below, these classifications overlap.
cels out and replaces the first edition.2 Following
are three key changes of the nine made:
• Three new reference standard sunscreens
have been validated and added (see Table 2);
Glass Particles to
• Sunscreen application procedures have been Boost SPF
described in greater detail; and
Check out Page 48 in the
• The reporting tables and requirements have April 2019 digital magazine.
been modified to provide
more complete informa-
tion on the results of Table 2. Reference Standard Sunscreens
the testing.
These changes will further
improve the accuracy of Reference Acceptance Limits
SPF determination. The new Sunscreen Mean SPF
Formulation Lower limit Upper limit
reference samples, SPF 30
(P5), SPF 43 (P6) and SPF P2 16.1 13.7 18.5
63 (P8), will especially allow P3 15.7 13.7 17.7
testing labs to check their
P5 30.6 23.7 34.4
equipment much closer to the
relevant market requirements. P6 43.0 31.0 54.9
Most countries have a cap of P8 63.1 43.9 82.3
SPF values in place, e.g., at

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CT2004_Testing_Osterwalder_irv.indd 43 3/18/20 1:51 PM

 Good as Gold

The ideal test alternative

would be accurate, agree
with in vivo results, show
improved reproducibility and
be easy to perform.

The ideal assessment method would be 1. In vitro

accurate and in agreement with in vivo results;
show improved reproducibility; and be easy to
perform—i.e., would be cost-effective. Below is
a brief summary of the alternative SPF methods
currently in discussion or under development;
some are already commercially available. They
are divided into three categories: 1) in vitro
transmission methods, 2) in silico methods and
3) hybrid diffuse reflectance spectroscopy. The
details of these methods can be found in the
indicated literature.
Transmission Methods
The in vitro transmission approach was the
first attempt to find an alternative to the in vivo
method. The first comparisons in vitro and in
vivo date back to over 40 years ago.10 While
many substrates have been attempted, the two
major requirements are: 1) transparency for UV,
and 2) a certain degree of roughness to mimic
the skin surface. Over the decades, polymethyl
methacrylate (PMMA) has been found to be a

Figure 2. SPF assessment methods

44 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Testing_Osterwalder_irv.indd 44 3/18/20 1:51 PM

 useful substrate, although other materials CE Method
have also recently been suggested.11 Sunscreen
Under the leadership of Cosmetics Europe
is applied to roughened PMMA plates that
(CE), a comparison of in vivo versus in vitro
attempt to mimic the texture of skin. Several
SPF test methods was conducted using 24
plates had been developed with different levels
commercial sunscreens, SPF 6-50+, in three
of roughness.
laboratories each. The CE method,15 developed
Transmission is measured by a spectropho-
by Miksa et al.,14 uses a robotic arm to control
tometer with an integrating sphere to catch
the spread of test products onto two different
scattered UV light. Together with the erythema
PMMA plates, molded and sandblasted. The
action spectrum and the (simulated) solar
CE method is currently a norm per the ISO
spectrum, the measured transmission data are
technical committee TC 217 (Cosmetics), under
then used to calculate the SPF. After several
the approved work item number and title:
decades of development, a working group
“ISO/AWI 23675 Cosmetics—Sun Protection
of the German Cosmetics Society concluded
Test Methods—In vitro Determination of Sun
the in vitro sun protection factor is still a
Protection Factor.”
challenge with no final answer,12 although a
recent breakthrough has been reported.13, 14
Three in vitro methods include: the Cosmetics
Europe (CE) Method;15 Fused Method;16 and C&T Sponsored Webcast Videos
other methods, e.g., JCIA method with “skin- Find current and upcoming webcasts at
www.CosmeticsandToiletries.com
mimicking substrate.”17

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | 45

CT2004_Testing_Osterwalder_fcx.indd 45 3/25/20 1:04 PM

 Good as Gold
Method includes in vivo DRS to assess UVA and in vitro ISO 24443 to assess UVB and photostability23
Figure 3. Experimental setup of H-DRS measurement
Fused Method
The “fused method” is the unofficial name of
a combination of different in vitro transmission
methods. A major new element is a calibration
step and the prediction of the “dispersal rate,”
after Batzer, et al.’s, “The 'Dispersal Rate'—A
Product Dependent Characteristic to Predict
the Reliability of the Calibrated in Vitro SPF on
WW5 Plates.”
In their work, the authors conclude:16 We sug-
gest implementing an individual calibration of the
in vitro SPF to improve the reproducibility of in
vitro SPF measurements between different labo-
ratories. Considering the Dispersal Rate helps to
estimate the reliability of the in vitro SPF measured
on WW5 plates. In order to evaluate whether those
products with a high Dispersal Rate can also be
calibrated with special standards, further mea-
surements need to be done. We demonstrate that,
besides the known parameter, also the composi-
tion of the products should be considered for the
interpretation of the in vitro SPF. Our findings
could explain some multiple reported problems
in correlation between in vitro and in vivo SPF,
especially for higher SPFs.
2. In silico Methods
Attempts to calculate the SPF and other per-
formance parameters of sunscreen started more
DM11 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Testing_Osterwalder_irv.indd 46
than 20 years ago. The state of the art is sum-
marized by Herzog and Osterwalder.18 In silico
is very similar to the in vitro transmission
method except the transmission measure-
ment through the roughened PMMA plate is
replaced by a calculation with a model of the
“non-uniform sunscreen” film on the skin.19
Then, it follows the same calculation as the in
vitro method. Commercial examples include
BASF’s “Sunscreen Simulator”20 and DSM’s
“Sunscreen Optimizer.”21
For market monitoring or surveys, the
simulator tool can be combined with UV filter
analysis, e.g., according to EN 17156.22 This
analysis then provides the UV filter concentra-
tions that can be plugged into the simulator.
Simulation tools are now freely available on
the internet.20, 21
In silico SPF determination methods are
becoming increasingly popular; they often pro-
vide realistic, usually rather conservative results.
In silico methods using the UV filter spectra of
sunscreens supplement the possibilities offered
by in vivo and in vitro methods. In silico calcula-
tion has, per se, no random error component
when repeating the “experiment.” This means
any deviation from the true SPF is systematic.
In silico SPF calculation also is being used by
authorities to monitor the market, e.g., CVUA
3/18/20 1:52 PM
 Karlsruhe, in Germany.23, 24 In the United States,
the in silico assessment of market products is
relatively easy since declaring the concentration
of UV filters on the packaging is mandatory.
Sun Protection Simulator
During the development of new sun
protection formulations, quick and inexpen-
sive methods for estimating UV screening
performance are highly desirable. The most
convenient approach toward this goal is given
by computational simulations, such as BASF’s
commercial “Sunscreen Simulator.” Models
for the calculation of SPF employ the same
algorithm used with in vitro SPF measurements
but replace the transmittance measurement
by calculating the overall absorbance of the
UV filters in an irregular sunscreen film. The
simulations require a database with quantitative
UV extinction spectra of the relevant UV filters,
as well as a mathematical description of the
film irregularity.
The simulation algorithm also implies the
consideration of photodegradation properties
of the UV filters in the sunscreen composition.
Besides using such simulations for designing
new sunscreen formulations, the calculations
can also support the understanding of sunscreen
performance in general.20
Sunscreen Formulation Tool
Another commercial sunscreen simulator
based on comparable mathematics has was
developed by DSM in 2017, the “Sunscreen Opti-
mizer.”21, 25 This in silico tool is also useful in the
development of sunscreens and UV protective
day care formulas. It functions like an in silico
laboratory and allows for the comparison of dif-
ferent formulation concepts in many aspects of
performance, as well as formulation parameters
such as oil load and oil UV filter content.
3. Hybrid Diffuse
Reflectance Spectroscopy
Hybrid diffuse reflectance spectroscopy
(HDRS or H-DRS) is based on non-invasive dif-
fuse reflectance spectroscopy (DRS). Here, UVA
protection (320-400 nm) is directly assessed in
vivo, and since the returning signal is not suf-
ficient in the UVB range (290-320 nm), the SPF
is calculated by extrapolating the UVA curve into
UVB by using in vitro data—which makes it a
hybrid method. Figure 3 provides a schematic
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Testing_Osterwalder_irv.indd 47
of the HDRS principle. Currently there are three
sub-types of HDRS: monochromatic,26 which is
commercially available; polychromatic,27 whose
rollout is anticipated; and multichromatic, LEDs,28
still under development.
The HDRS methods are currently developed
into a norm in the ISO technical committee TC 217
(Cosmetics), under the approved work item number
and title: ISO/AWI 23698, “Cosmetics Sun Protec-
tion Test Methods—Measurement of the Sunscreen
Efficacy by Diffuse Reflectance Spectroscopy.”
HDRS, Monochromatic
The HDRS concept has been developed in the
U.S. by Ruvolo, et al.—the first DRS in 2009, for
the determination of UVA-PF;29 then in 2014, for
SPF determination.30 Its further development to
a commercial method was a multinational effort
lead by Rohr, et al.,26 in Germany, with equipment
from Bentham, UK. So far, hundreds of samples
have been measured by HDRS. The UVA-PF and
SPF values appear to be in good agreement with
in vitro and in vivo UVA values after ISO 24443
and ISO 24442, and the SPF gold standard
ISO 24444, respectively.
HDRS, Polychromatic
The Solar Light Company has built a polychro-
matic HDRS version27 that measures an integral
signal of the UVA part, combined with a full
spectrum in vitro scan, and thus has a simpler opti-
cal and mechanical design. Tests can be conducted
in a shorter time frame versus a monochromatic
device that must scan the spectrum one wavelength
at a time.
HDRS, Multichromatic, LEDs
Another approach using the HDRS principle
was developed at the Charité in Berlin, together
with Courage-Khazaka, Cologne.28 Here, to further
reduce the complexity of the equipment, LEDs
are used as a light source. The first prototype
used an LED at 310 nm, which is surprising since
UVB is practically not reflected. The latest ver-
sion uses eight LEDs spread over the whole UVB
UV Imaging Uncovers
Sun Protection
Click to Page 33 in the
September 2019 digital magazine.
| DM12
3/18/20 1:52 PM
 Good as Gold

the gold standard. So far, none of the alterna-

Validation must predict tives is completely free from flaws but many
hold promise for attempting validation against
what will happen with the ISO 24444.

new method after it is Validating Alternative

released for general use.
and UVA range. This technology is still in the
research and development stage but deserves
close attention.
Overview of Replacement
Test Methods
Pressure to replace the current gold standard
is increasing, due to the availability of alterna-
tive methods and the engagement of their
supporters. Table 3 provides an overview of the
status of alternative methods, compared with
SPF Methods
Before an alternative method can replace
an existing one, it must be compared with the
standard. Basic principles and guidelines for
validation can be found in ISO Norm 5725:
“Accuracy (Trueness and Precision) of Measure-
ment Methods and Results.”31 Trueness refers to
the closeness of agreement between the arith-
metic mean of a sufficient number of test results
and the true. Precision refers to the closeness of
agreement between the test results.
Validation involves more than simply a cor-
relation between two data sets. For the latter, a
direct plot often is utilized, and the square of the
correlation coefficient can be used as a correla-
tion quality parameter. However, this approach

Table 3. Status of Sunscreen Test Methods

Method Type ISO Status Method Description Evolution, Characteristics, Properties

ISO Biological endpoint, complex method,
Gold Standard
In vivo 24444:2019 relevant for skin cancer
Diffuse Reflectance Combines in vivo and in vitro method,
H-DRS
Spectroscopy + holds potential to replace all current
ISO/AWI 23698
ISO 24443 methods
In vitro Forty years of development, good to
Transmission PMMA plates transmission,
assess incremental improvements, not
ISO/AWI 23675 automated application
universal (skin/plastic)
Calculated UV filter spectra + irregular Steady improvement over past 20 years,
In silico (no ISO status) skin-film model + popular for sunscreen development and
EN 17156 market monitoring

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 can be misleading. A Lancet paper by Bland and
Altman32 warns about drawbacks and suggests
another way of comparing the data utilizing a
Bland-Altman plot. Such correlation plots com-
bined with inclusion/exclusion criteria require,
depending on the variability of the two methods
being compared, a significant amount of data
input to reach a validation decision that is not
strongly influenced by random data fluctuations.
Validation must predict what will happen
with the new method after it is released for
general use. Therefore, one must go beyond the
Bland-Altman analysis. Some key features that
impact the accuracy and variability of results of
the new method should be known and under-
stood. These include:
• The random variability, i.e., an error that
cannot be controlled by the procedure;
• The systematic method bias, i.e., a con-
stant deviation from the standard method;
• The sample-specific variation or matrix
component—an error that this specific to a
sample or a group of samples and does not
average out by retesting; and
• Any laboratory-specific bias.
The matrix component could neutralize
itself when looking at overall data samples
but it is crucial to monitor this, as it can-
not be corrected through parametrization
Figure 4. Evolution of validation process for the agreement of two methods
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Testing_Osterwalder_irv.indd 49
and can make a method particularly wrong.
For example, the in silico methods do not
show random variability; however, the key
trueness-defining parameter comes down to the
sample-specific component.
It is also important to know the reproduc-
ibility and repeatability of the new method.
A “Variance Component Model” can reveal
these parameters. Combined with a factorial-
fractional-design that would test not all, but
sufficient possible conditions, such a model
can prove to save on costs. Figure 4 shows the
evolution of the validation process.
Interlaboratory Study Design
It also is not possible to adequately char-
acterize and assess the performance of an
alternative method against the gold standard
if any observed error is not partitioned into
different components; e.g., laboratory bias,
repeatability error, etc., described above. This
will correctly align errors with their respective
underlying causes.
For instance, if overall bias is negligible
but a laboratory bias affects the gold standard
results, individual differences can correctly be
interpreted as caused by laboratory bias and
affecting only the gold standard. As another
example, for in silico methods there is neither a
repeatability error nor a laboratory bias; how-
| DM14
3/18/20 1:52 PM
 Good as Gold
ever, the preliminary determination of absorption
values may have been subject to errors.
Take the case that for a given ingredient, A,
the absorption value in the in silico method’s
reference database has a negative bias. Then, all
products that contain a certain amount of for-
mulation ingredient A would be affected by this
negative bias. This illustrates why the distinction
between different sources of error is important to
correctly characterize method performance.
To put it succinctly: in many cases, and
particularly if both the gold standard and the
alternative method display considerable varia-
tion, a correct characterization and assessment
of method performance is not possible without
breaking down the observed error. Figure 5 illus-
trates how the difference sources of error may
affect SPF results on the basis of hypothetical
data but with realistic relative dispersion values.
Proposed Validation Method
Accordingly, herein it is proposed to imple-
ment an experimental design that allows for the
adequate characterization of the effects associ-
ated with laboratories, products and repeatability
error. More specifically, it is proposed the test
design should include three different product
types to cover formulations comprised of one
phase, two phases more than two phases; and
that for each product type, three different SPF
levels, i.e., 15, 30 and 50+, should be considered,
resulting in nine total product groups. Finally,
for each product group, it is proposed to include
four different products, in order to strike a
balance between statistical requirements and
cost efficiency.
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CT2004_Testing_Osterwalder_fcx.indd 50
Since such a test design can result in a consid-
erable workload, great attention has been given
to the efficiency of this design. In particular, the
use of orthogonal designs, as described by Uhlig
and Gowik,33 allows for the reliable estimation of
different components of variability while ensur-
ing economy of resources and with as few as four
participating laboratories per method.
Hand-in-hand with this experimental design,
the use of a so-called mixed linear model will
allow the different bias and precision estimates
to be calculated: repeatability error, overall bias,
laboratory-specific bias and product bias. Mixed
linear models will allow a characterization of the
variation between laboratory and product bias
values to be characterized. Indeed, while both
laboratory bias and product bias are interesting
as individual positive or negative values affecting
a given laboratory or product, it is equally infor-
mative to look at the variation across bias values.
In other words, in method validation, it is
often useful to characterize product or labora-
tory bias as a standard deviation—just as in
the case of repeatability error. The between-
laboratory standard deviation can then be used
to predict expected variations in bias when SPF
is determined for one and the same product
in different laboratories. Concurrently, the
between-product standard deviation can be used
to predict expected variation in bias when SPF is
determined for different products in one and the
same laboratory.
The Way Forward
Over the past decades, many alternative
methods attempting to replace ISO 24444 SPF in
vivo have been developed and are currently being
optimized. In silico and in vitro methods appear
attractive as they can be performed without
human subjects. These methods have also proven
useful as prediction tools in the planning and
development phase for new sunscreens. HDRS is
another alternative method based on an interest-
ing hybrid approach.34
Will a non-human sun protection method ever
succeed for labeling purposes, or is the human
skin component an unavoidable condition? The
next validation steps will provide some answers.
In the meantime, it is recommended to leverage
the entire SPF testing toolbox by performing
all of the methods outlined, thus ensuring
consumer safety.
3/25/20 1:50 PM
 a)

b)

Per product, eight labs submitted duplicate results (shown as matching pairs of symbols). Boxes = mean ± one reproducibility
standard deviation (SD) for each product. Corresponding mean values across labs for the gold standard are shown as horizontal
red lines. Clearly, for some products, the alternative method had a negative bias (e.g., Product C), while for others, a positive bias
(e.g., Product B). The dispersion of the alternative method results can be quite low (e.g., Product C) or quite high (e.g., Product J).
The dispersion for a given product has only two main components—repeatability and between-lab variability—but variations
across products themselves constitute a third component. With product J, e.g., both repeatability and between-lab components are
large, whereas product bias is small.

Figure 5. SPF values obtained by alternative method for 12 test products A-L (top), and
corresponding difference between alternative and standard, ln(ALT) and ln(REF) (bottom)

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | DM16

CT2004_Testing_Osterwalder_irv.indd 51 3/18/20 1:52 PM

 Good as Gold

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performance. Pure Appl Chem.
1. Osterwalder U., Schütz, R. and Vollhardt J. (2018, Apr 13). SPF
assessment revisited–status and outlook. SOFW, 144. 19. Ferrero, L., Pissavini, M., Marguerie, S. and Zastrow, L. (2003).
Efficiency of a continuous height distribution model of sunscreen
2. ISO. (2010). Sun protection test methods: In vivo determination
film geometry to predict realistic sun protection factors. J
of the sun protection factor (SPF). ISO 24444:2010, Cosmetics.
Cosmet Sci, 54, 463-481, (2003)
https://www.iso.org/standard/46523.html
20. BASF website. (accessed on 2020, Feb 16). Sunscreen
3. ISO. (2019, Dec). Sun protection test methods: In vivo determi-
Simulator. https://www.sunscreensimulator.basf.com/
nation of the sun protection factor (SPF). ISO 24444:2019(E),
Sunscreen_Simulator/computation
Cosmetics, 2nd edn. https://www.iso.org/standard/72250.html.
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www.sunscreen-optimizer.com
Edinger, C. (2015). Revisiting human skin, sunscreen films
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Protection Conference/London. cosmetic products of the 22 organic UV filters in use in the EU.
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5. Adlhart, C., Edelmann, M. ... Vollhardt, J., et al. (2017).
Distribution differences of individual UV filters related to applica- 23. Mildau, G. (2015, May). Aktuellen stand der amtlichen beur-
tion procedure and substrate probed by Raman confocal teilung von sonnenschutzcremes in Europa. (Current status of
microscopy. Proceedings: 14th International Sun Protection the official assessment of sun protection creams in Europe). In:
Conference/London. Schmidt-Lewerkühne, H., Mensch & Sonne, DGK Symposium.
Kongresszentrum Darmstadium, Darmstadt. SÖFW J 141,
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11/15.
Labeling and effectiveness testing; Sunscreen drug products
for over-the-counter human use. Federal Register, 76(117), 24. CVUA Karlsruhe, Germany. (2020, Mar 9). https://www.ua-bw.
35620-35665. de/pub/default.asp?subid=2&Lang=DE
7. Garzarella, K. and Caswell, M. (2013). Disparate SPF testing 25. Osterwalder, U., Janssen, A. and Schlifke, A. (2018). A new
methodologies generate similar SPFs. J Cosmet Sci, 64, option for SPF assessment? COSSMA 1-2, 20-24. https://
297–307 (2013). www.cossma.com/ingredients/article/a-new-option-for-spf-
assessment-35315.html
8. Alejandria, M., Marra, A., Roberts, G. and Caswell, M. (2019,
Jul/Aug). Disparate SPF testing methodologies generate similar 26. Rohr, M., Ernst, N. and Schrader, A. (2018, May 23 e-pub).
SPFs. II. Analysis of P2 standard control SPF data. J Cosmet Hybrid diffuse reflectance spectroscopy: Non-erythemal in vivo
Sci, 70(4), 181-196. testing of sun protection factor. Skin Pharmacol Physiol, 31(4),
220-228. doi: 10.1159/000488249. PMID:29791917.
9. Miksa, S., Lutz, D., Guy, C. and Delamour, E. (2016, Dec).
Sunscreen sun protection factor claim based on in vivo inter- 27. Cole, C., Silverman, J. and Bonitatibus, M. (2019). Evaluating
laboratory variability. Int J Cosmet Sci, 38(6), 541-549. sunscreen ultraviolet protection using a polychromatic diffuse
reflectance device. Photodermatol Photoimmunol Photomed,
10. Sayre, R.M., Agin, P.P., LeVee, G.J. and Marlowe, E. (1979,
35(6), 436–441. doi:10.1111/phpp.12496.
Mar). A comparison of in vivo and in vitro testing of sunscreen-
ing formulas. Photochem Photobiol, 29(3), 559-66. 28. Reble, C., Gersonde, I., Schanzer, S., Meinke, M.C., Helfmann,
J. and Lademann, J. (2018). Evaluation of detection distance-
11. Sohn, M., Malburet, C., Baptiste, L. and Prigl, Y. (2017, May
dependent reflectance spectroscopy for the determination of the
24). Development of a synthetic substrate for the in vitro per-
sun protection factor using pig ear skin. J Biophotonics, 11(1),
formance testing of sunscreens. Skin Pharmacol Physiol, 30(3),
10.1002/jbio.201600257. doi:10.1002/jbio.201600257.
159-170. doi: 10.1159/000464471.
29. Ruvolo E., Jr., Chu, M., Grossman, F., Cole, C. and Kollias, N.
12. Rohr, M., Klette, E., ... Zastrow, L., et al. (2010, Mar 9). In vitro
(2009). Diffuse reflectance spectroscopy for ultraviolet A protec-
sun protection factor: Still a challenge with no final answer. Skin
tion factor measurement: Correlation studies between in vitro
Pharmacol Physiol, 23(4), 201-12. doi: 10.1159/000292777.
and in vivo measurements. Photodermatol Photoimmunol Pho-
PMID: 20215813.
tomed, 25(6), 298-304. doi:10.1111/j.1600-0781.2009.00469.x.
13. Miksa, S., Lutz, D. and Guy, C. (2015). New approach for a
30. Ruvolo, E., Col,e C. and Kollias, N. (2014). New noninvasive
reliable in vitro sun protection factor method-Part I: Principle
approach assessing in vivo sun protection factor (SPF) using
and mathematical aspects. Int J Cosmet Sci, 37(6), 555–566.
diffuse reflectance spectroscopy (DRS) and in vitro transmission.
doi:10.1111/ics.12226.
Photodermatol Photoimmunol Photomed, 30(4), 202-11.
14. Miksa, S., Lutz, D., Guy, C. and Delamour, E. (2016, May 6
31. ISO. (1994, Dec 15). ISO 5725-1:1994(en), Accuracy (trueness
e-pub). New approach for a reliable in vitro sun protection factor
and precision) of measurement methods and results–Part 1:
method-Part II: Practical aspects and implementations. Int J
General principles and definitions, ...–Part 6: Use in practice of
Cosmet Sci (2016, Oct), 38(5) 504-11. doi: 10.1111/ics.12327.
accuracy values. International Standard, 1st edn.
PMID: 27060786.
32. Bland, J.M. and Altman, D.G. (1986). Statistical methods for
15. Pissavini, M., Tricaud, C., ... Matts, P.J., et al. (2018, Apr 20
assessing agreement between two methods of clinical measure-
e-pub). Validation of an in vitro sun protection factor (SPF)
ments. Lancet, i:307-316.
method in blinded ring testing. Int J Cosmet Sci, 10.1111/
ics.12459. doi: 10.1111/ics.12459. PMID: 29676800. 33. Uhlig, S. and Gowik, P. (2018). Efficient estimation of interlabora-
tory and in-house reproducibility standard deviation in factorial
16. Batzer, J., Bleckmann, A., Lerg, H., Schwanke, F. and Schläger,
validation studies. J Consumer Protection and Food Safety,
T. (2016). The 'Dispersal Rate'-A product dependent charac-
https://doi.org/10.1007/s00003-018-1157-x
teristic to predict the reliability of the calibrated in vitro SPF on
WW5 plates. Int J Cosmet Sci, 38(3), 294–304. doi:10.1111/ 34. Ruvolo, E., Aeschliman, L. and Cole, C. (2020, Feb 6 e-pub).
ics.12293. Evaluation of sunscreen efficacy over time and re-application
using hybrid diffuse reflectance spectroscopy. Photodermatol
17. Miura, Y., Takiguchi, Y., ... Shirao, M. et al. (2008). Algorithm for
Photoimmunol Photomed, 2020, 10.1111/phpp.12535.
in vitro sun protection factor based on transmission spectrum
measurement with concomitant evaluation of photostability.
Photochemistry and Photobiology, 84, 1569-75.

DM17 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Testing_Osterwalder_irv.indd 52 3/18/20 1:52 PM

 CONCEPT DEVELOPMENT CONSUMER

The only event giving

you tools to streamline
beauty product development
from concept to consumer.
October 13-14, 2020
Pre-register today
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 Testing | C&T ®

KEY POINTS
• The ISO sets proposed standards
and test methods for nearly
every industry; its validation
process is described here.

• In addition, methods
under review pertaining
to sun protection
are discussed.

Peer-reviewed

Reproduction in English or any other language of

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© 2020 Allured Business Media.

CT2004_Testing_Pissavini_fcx.indd 46 3/23/20 10:07 AM

 STANDARDIZING
SAFETY ISO Validation and Sun Protection Tests
facebook.com/CandTmagazine Marc Pissavini, Ph.D.
International Organization for Standardization (ISO),
Cosmetics & Toiletries TC217/WG7 Convenor
Coty-Lancaster, Monaco
@cosmeticsandtoiletries

T he International Organization
for Standardization (ISO) is
the world’s largest developer
of voluntary international
standards. This non-gov-
ernmental international
organization was founded in 1947. Today, ISO
has members from 164 countries and nearly
160 individuals work full time for the Central
Secretariat in Geneva, Switzerland. Through
its members, the group brings together
experts to share knowledge and develop
voluntary, consensus-based, market-rele-
vant international standards that support
innovation and provide solutions to global
challenges. It is important to note that
ISO does not carry out certification of
conformity to its standards.
ISO has published more than 23,000
international standards and related
documents covering almost every
industry, from technology and food
safety, to agriculture and health care.
ISO Working Group 7 (WG7), "Sun

Reproduction in English or any other language of all or part of this article is strictly prohibited. © 2020 Allured Business Media. Cosmetics & Toiletries® | 47

CT2004_Testing_Pissavini_fcx.indd 47 3/18/20 2:04 PM

 Standardizing Safety
Even if globally the cosmetic industry used
the water resistance claim,
no ISO method yet exists for it.
Protection Test Methods," was established in 2006,
but the latest improvements were launched in
2016 through a systematic review of in vivo SPF,
followed in 2017 by the in vivo and in vitro UVA
methods. At the same time (2016), the valida-
tion process of in vivo water resistance began.
During the ISO meeting at the end of 2018, two
new alternative SPF methods—hybrid diffuse
reflectance spectroscopy (HDRS) and the SPF in
vitro double approach—were approved as new
work items. At the end of 2019, when this paper
was written, seven methods were undergoing
standardization processes and three of them were
close to the publication.
The present paper describes the ISO stages
for the review and validation of standards. It also
gives an overview of current and pending methods
pertinent to sunscreen testing.
ISO Structure and Function
As stated, the ISO organization consists of
a network of national standards bodies, the
most representative of standardization in each
country, from all regions of the world, working
in partnership with international organizations.
In 1951, the group published its first standard/
recommendation, ISO/R 1:1951, “Standard
reference temperature for industrial length mea-
surements.” Since then, this standard has been
updated numerous times and has now become,
“ISO 1:2002 Geometrical Product Specifications
(GPS)—Standard reference temperature for geo-
metrical product specification.”
The worldwide market for sunscreen creams
is expected to rise with a CAGR of ~4.9%
from 2019-2024, reaching US $10.79 billion in
2024, up from ~$85 billion in 2019.
Source: Industry Research
48 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Testing_Pissavini_fcx.indd 48
Within ISO, experts form a technical commit-
tee that is responsible for a specific subject area.
For example, in 1998, ISO Technical Committee
(TC) 217, “Cosmetics,” was created by Iran, which
still holds the secretariat. Today, this TC includes
41 participating countries and 28 observing
countries, subdivided into four working groups
(WG) (see Figures 1 and 2):
WG1: Microbiological standards and limits
WG3: Analytical methods
WG4: Terminology
WG7: Sun protection test methods
At the European level, a similar structure is in
place (see Figure 2) although the “WG” terminol-
ogy is not present.
7 Steps to ISO Validation
There are seven main stages of development
for the ISO validation process:
1. Pre-work Item (PWI)
2. New Work Item Proposal (NWIP)
3. Working Draft (WD) or preparatory stage
4. Committee Draft (CD)
5. Draft Internal Standard (DIS)
6. Final Draft International Standard (FDIS)
7. Publication
Two of these are optional—i.e., the PWI and
CD stages. Technical and editorial comments can
be made throughout and up until the FDIS stage
in order to improve the document. At the FDIS
stage, only editorial comments are allowed. The
publication of a norm typically takes three years
but can be extended to four.
WG 7: Sun Protection
Test Methods
As stated, within ISO, WG7 “Sun Protec-
tion Test Methods” was set up in 2006 and
since then, much standardization work has
been accomplished.
SPF In vivo, ISO 24444: In 2010, the first ISO
norm, “SPF In vivo” (ISO 24444), was published
by WG7. This norm is accepted today as a gold
3/18/20 2:04 PM
 standard around the world (except in the United
States) to claim SPF. It recently underwent a
systematic review process to improve the method
and reduce the inter-lab variability of results.
Therefore, if you repeat the test with the updated
version, the mean value will not change. The
main updates concern the application techniques,
addition of new standards with higher SPF values,
control of the lamp beam uniformity, and better
precision of the rejected cases. The method was
finalized and published in February 2020. For
more on these changes, see Page 43.
UVA In vivo, ISO 24442: One year later, in
2011, ISO published the “UVA In vivo” method
ISO 24442. Similar to the ISO 244444, this
method is currently under a systematic review

Figure 1. ISO/TC217 participating countries

Figure 2. Structure of ISO/TC 217 compared with European CEN/TC 392; examples
of national standards bodies

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | 49

CT2004_Testing_Pissavini_fcx.indd 49 3/18/20 2:04 PM

 Standardizing Safety

Figure 3. Different stages during the development of an ISO norm

process in order to improve the method and
reduce the inter-lab variability of results. This
method being technically close to the SPF
In vivo, the improvements are similar and
will be harmonized with the ISO 24444. This
method should be published at the end of 2021.
UVA In vitro, ISO 2443: The last method
under systematic review is the “UVA In vitro”
method ISO 24443. This method was published
in 2012 will be optimized thanks to different
modifications, such as the addition of a high
UVA protection factor standard value; a more
precise application protocol; the possibility to
used sandblasted plates as substrates, etc. Cur-
rently in the CD stage, ISO 24443 is targeted for
revision and publication by the end of 2020.
Water Resistance
Even if globally the cosmetic industry used
the water resistance claim, no ISO method yet
exists for it. In 2015, WG7 launched a new work
item, ISO 16217, for a water immersion proce-
dure. This new method is, in fact, somewhat of
a mix between the existing U.S. Food and Drug
Administration (FDA) and Colipa methods.
Many improvements and harmonization with

Figure 4. Seven different ISO norms currently under development

50 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Testing_Pissavini_fcx.indd 50 3/18/20 2:04 PM


the In vivo SPF ISO 24444 are scheduled
for ISO 16217. As of press, it is currently
in the FDIS stage and its target date for
publication is the beginning of 2020.
Linked to the immersion procedure is
ISO 18861, for the determination of the
percentage of water resistance, which
has been under development since 2016.
This method will only be implemented by
countries utilizing a percentage to claim
the water resistance of the sunscreen
product, and not the SPF after-bath as is
claimed in the United States. The target
date for this publication is summer 2020.
In vitro Efforts
The European Commission, as well as
health associations and non-governmental
organizations, recommends that the
industry increase efforts toward the
development of in vitro test methods
to deliver results equivalent to the ISO
24444 for protection against erythema.1
Two new works were launched in 2018
to fill this gap since, surprisingly—and
despite some reports—to date, no in
vitro or in silico SPF determination is
internationally validated.
Hybrid diffuse reflectance spectros-
copy: The first method, hybrid diffuse
reflectance spectroscopy (HDRS), is not a
100% in vitro procedure; it is for this rea-
son it is called a hybrid. Basically, in order
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Testing_Pissavini_fcx.indd 51
In vitro test methods are
needed to deliver results
equal to the ISO 24444
for protection against
erythema.
to obtain a full UV absorption spectrum, the in
vitro absorbance must be scaled to match the
in vivo diffuse reflectance spectroscopy (DRS)
absorbance values. Then, the UVB in vitro
portion must be mathematically attached to the
UVA portion from the In vivo DRS technique.2
This hybrid method is currently under discus-
sion by experts in WG7 and the target date for
publication is at the end of 2021. For more on
this method, see Page 40 in this issue.
Purely in vitro measurements to determine
a product’s sun protection factor (SPF) have
been attempted for decades. By the end of the
1970s, tests were carried out on various artificial
supports; and in the 80s and 90s, a multitude of
publications tried to correlate the results of in
vivo SPF tests with in vitro results, with more or
less success.
CE SPF In vitro method: Cosmetics Europe
(CE), having developed the UVA In vitro method
in 2007 that is used to validate ISO 24443,3
decided in 2016 to focus its efforts on the
development and validation of in vitro SPF.
However, one of the problems encountered
by all attempts at validation—which, in turn,
UV Imaging Uncovers
Sun Protection
Check out Page 33 in the
September 2019 digital magazine.
| 51
3/18/20 2:04 PM
 Standardizing Safety
The European Commission
urges the industry to
develop new in vitro tests
equal to ISO 24444.
delayed the acceptance of this method—was
that precisely no validation criteria existed for
sun protection factors.
In 2017, WG7 proposed and recommended
the use of sufficiently precise and relevant
acceptance criteria for CE to launch a valida-
tion program. CE therefore blind-tested 24
VIDEO
52 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Testing_Pissavini_fcx.indd 52
emulsions with a claimed SPF of between 6 and
50+; i.e., the claimed SPFs were unknown by
the evaluating institutes or laboratories. Tests
were performed in three European institutes for
the SPF In vivo, using the ISO 24444 standard;
and in three European laboratories for the SPF
In vitro, using a new method developed by CE.
This SPF In vitro method, ISO/TC 217, is the
result of years of development by experts under
the leadership of CE and refined by an ISO
ad hoc group.4
As previously reported (see video: Novel
In vitro SPF Test Method Validated),
Validated
regression analysis revealed a strong correla-
tion between in vitro and in vivo values (p <
0.0001).5 The ISO “acceptance criteria funnel”
defines upper and lower confidence intervals
at 95%. Thus, the results from this blinded
ring study showed that data from the paired in
vivo and in vitro SPF tests fit well within ISO
acceptance criteria.
Recently, 76 products were added to the cor-
relation. This CE-validated method is currently
in a working draft 4 stage and is under discus-
sion by the experts of WG7. The target date
for publication is at the end of 2021. Figure 4
depicts the seven different norms currently
under development, all at different stages.
Conclusion
ISO was founded with the goal to answer
one fundamental question: What's the best way
of doing this? It started with obvious things
like weights and measures, and over the last 50
years, it has developed into a family of stan-
dards that covers everything from the shoes we
stand in, to the Wi-Fi networks that connect us
invisibly to each other.
Addressing all of these and more, interna-
tional standards give consumers confidence that
their products are safe, reliable and of good
3/25/20 11:44 AM
 quality.6 ISO's standards for SPF, UVA and/or
water resistance are just a few examples that help
to make the world a safer place. To date, seven
methods are undergoing standardization process:
• Three are under systematic review and will
not require the retesting of products with the
updated version; and
• Four are new methods that, no doubt, will help
the cosmetics community with the addition of
new standardized methods for calculating the
percentage of water resistance and carrying
out immersion procedures, or by proposing
alternative methods to the ISO 24444 SPF
In vivo method.
All of these standardized methods will be
published within the next two years, greatly
improving sun product efficacy. Furthermore,
regulators and governments rely on ISO WG7
standards to help develop better regulations,
knowing they have a sound basis thanks to the
involvement of globally established experts—to
whom the author extends his thanks.
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Testing_Pissavini_fcx.indd 53
References
1. Document 32006H0647. Commission Recommendation of
22 September 2006 on the efficacy of sunscreen products
and the claims made relating thereto (notified under docu-
ment number C(2006) 4089) (Text with EEA relevance).
(2006, Sep 22). Retrieved from https://eur-lex.europa.eu/
legal-content/EN/TXT/?uri=CELEX:32006H0647
2. Ruvolo, E., Jr., Kollias, N. and Cole, C. ( 2014). New non-
invasive approach assessing in vivo sun protection factor
(SPF) using diffuse reflectance spectroscopy (DRS) and in
vitro transmission. Photodermatol Photoimmunol Photomed
30 202-211.
3. Matts, P.J., Alard, V., ... Wolber, R., et al. (2010). The Colipa
in vitro UVA method: A standard and reproducible measure
of sunscreen UVA protection. Int J Cosm Sci 32 35-46.
4. Pissavini, M., Tricaud, C., ... Matts, P.J., et al. (2018).
Validation of an in vitro sun protection factor (SPF) method
in blinded ring-testing. Intl J Cos Sci
5. Pissavini, M. (2019, Mar 14). [video] Novel in vitro
SPF test method validated. Cosm & Toil. Retrieved
from: https://www.cosmeticsandtoiletries.com/testing/
methoddevelopment/video-Novel-In-vitro-SPF-Test-
Method-Validated-507153681.html
6. ISO website (2020, Accessed Feb 24). Benefits of
standards. Retrieved from https://www.iso.org/benefits-of-
standards.html
| 53
3/18/20 2:04 PM
 Formulating | C&T ®

KEY POINTS
• Lasting deodorant efficacy may be achieved
without impacting the natural human
axillary microbiome.

• Here, 2-methyl 5-cyclohexylpentanol is

explored for its deodorant efficacy and
impact on the human axillary microbiome,
and compared with triclosan.

facebook.com/CandTmagazine

Cosmetics & Toiletries

@cosmeticsandtoiletries

Reproduction in English or any other language of

54 | www.CosmeticsandToiletries.com all or part of this article is strictly prohibited. Vol. 135, No. 4 | April 2020
© 2020 Allured Business Media.

CT2003_Formulating_Genrich_fcx.indd 54 3/20/20 2:22 PM

 Mind
Your
Microbes
Supports the Axillary Microbiome
T
he formation of
body odor begins
with odorless
human sweat
that is mainly
composed
of water, but also contains small fractions of
proteins and natural lipids. Natural skin micro-
biota will decompose such lipids and proteins
to form molecules with a particularly low odor
threshold. These molecules may include short
chain fatty acids, such as 3-hydroxy-3-methyl-
hexanoic acid (HMHA) or 3-methyl-2-hexenoic acid
(3M2H); as well as organosulfur compounds, e.g.,
3-mercapto-3-methyl-1-hexanol; even steroids such
as androstenol or androstenone may be present.1
Managing body odor is typically achieved via
Reproduction in English or any other language of all or part of this article is strictly prohibited. © 2020 Allured Business Media.
CT2003_Formulating_Genrich_fcx.indd 55
Gentle Malodor Protection
Florian Genrich, Ph.D., Steffen Nordzieke, Ph.D.,
Christin Koch, Ph.D., and Gerhard Schmaus, Ph.D.
Symrise AG, Holzminden, Germany
Sabrina Behnke, Ph.D.
Symrise Inc., Teterboro, NJ, USA
three approaches, used separately or in combination:
antiperspirants, deodorant actives and/or odor-masking
agents. Deodorant actives, in particular, typically are
used either to deodorize without the use of aluminum
salts (antiperspirants), or to deodorize with low or no
fragrance. Applying such actives in combination with
other technologies can support lasting odor protection,
which is what consumers expect from the ideal deodor-
ant product.2
Deodorant actives mainly function as antimicrobi-
als, selectively targeting the natural skin microbiota
that decompose lipids and proteins and cause odor;
for example, the antimicrobial triclosan, which often
is used as the benchmark with which to compare
modern actives. Triclosan represents a conventional
organohalogen, i.e., organochlorine system; alternative
non-organohalogen technologies include cosmetic
Cosmetics & Toiletries® | 55
3/20/20 2:22 PM
 Mind Your Microbes
Triclosan had a significant impact on the
microbiome composition, causing a significant
shift. 2-Methyl 5-cyclohexylpentanol, on the
other hand, had very low influence.
Biofilms and the
Skin Microbiome
Check out Page 30 in the
January 2020 digital magazine.
ingredients such as farnesol,3 triethyl citrate4
and 2-methyl 5-cyclohexylpentanola.5-7
However, recent emphasis on the skin micro-
biome has underlined a lack of information
about the impact of antimicrobial ingredients
on the natural axillary microbiome.8, 9 As such,
an ex vivo model10 was developed to uncover the
influence of deodorant actives on the human
axillary microbiome.11
The present article compares the effects of
modern and conventional deodorant actives, i.e.,
2-methyl 5-cyclohexylpentanol and triclosan,
respectively, on the axillary microbiome. As a
first step, the deodorizing performance of both
actives was demonstrated in two clinical sniff
tests. In the second step, researchers looked
in greater depth at microbial levels, as well as
the relative abundance of natural microbiota,
by applying the novel ex vivo human axillary
microbiome model.10
Experimental Design
Two in vivo clinical studies on human
subjects were carried out, comparing armpits
a
SymDeoB125 (INCI: 2-Methyl 5-Cyclohexylpentanol),
Symrise
The global antiperspirant and deodorant
market is expected to register a CAGR of 3.5%
between 2019 and 2024 to reach
US $70 billion.
Source: Market Research Future
56 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2003_Formulating_Genrich_fcx.indd 56
treated with 2-methyl 5-cyclohexylpentanol and
triclosan, as well as untreated armpits. Evalua-
tions were made by direct olfactory assessment
(sniffing), as well as self-assessment by the
subjects. The individual actives were applied
using a volatile carrier system (pump spray).
2-methyl 5-cyclohexylpentanol vs. triclo-
san, 24-hr clinical: As stated, an olfactory
assessment for malodor reductionb by each of
the test products was carried out comparing
them with one another and to the initial value.
The assessment was conducted in a random-
ized, double-blind, half-side manner in the
armpits of 20 subjects, ages 29 to 63 years, with
distinct perspiration odor in the armpit.
The study began with a ten-day conditioning
period during which subjects were only allowed
to use unscented soap without antibacterial
ingredients, and also excluding the use of anti-
perspirants, deodorants or other cosmetics. The
subjects were instructed to wear clothing not
treated with perfumed detergent or softener,
and only subjects with an odor score of no less
than 3, on a 0-5 scale (0 = no odor, 5 = very high
odor), were allowed to take part in the study.
After the conditioning period, 6 hr after
washing and 24 hr after washing (t0 = no
product applied), a sniff assessment of the
subjects’ armpits was performed by trained
experts to establish the control. Next, half of
the volunteers applied test formula A (2-methyl
5-cyclohexylpentanol spray) in the left armpit
and formula B (triclosan) in the right (see
Formula 1); the other volunteers applied the
test products in the reverse order. After this
single application, 6 hr and 24 hr later, sniffing
assessments were again performed (t1 = single
application). After the 24-hr assessment, sub-
jects applied the test products in the morning
and evening for four additional days, ending in
one last application on the morning of the fifth
day. Again, 6 hr and 24 hr after the last applica-
b
Institute Dr. Schrader in Holzminden, Germany
3/20/20 2:22 PM
 tion, sniffing assessments were performed (t11 = direct sniffing/olfactory assessment of the arm-
11 applications in total). pits by three trained assessors per the sensory
2-methyl 5-cyclohexylpentanol vs. untreated, olfactory method ASTM E1207-14 Standard
48-hr clinical: Sensory evaluation of the clinical Guide for Sensory Evaluation of Deodorancy.
efficacyc of the 2-methyl 5-cyclohexylpentanol The sniffing results were rated on a 10-point
deodorant versus untreated armpits also was con- scale from 0 (no bad odor) to 10 (extremely
ducted. In this case, sniff test assessments were strong odor).
made at 6 hr, 24 hr and 48 hr after the last appli- Thirty subjects, ages 29 to 60 years (mean
cation to the underarms of research subjects. age 50 ± 9), took part in this study. It began with
The assessment compared the left versus right a 7-day conditioning phase in which the subjects
armpit, with the product applied on the left and used only a neutral soap (cleaning agent)
only washing on the right, or vice versa. The test supplied by the institute, having no bacteri-
product was in the form of
a simple alcoholic pump
Formula 1. Test Deodorant Sprays
spray comprising ethanol
(96%) at 99.7% w/w and
0.3% w/w of 2-methyl A (% w/w) B (% w/w)
5-cyclohexylpentanol. Ethanol, 96% 39.7 39.7
Axillary odor was 2-Methyl 5-Cyclohexylpentanol 0.3 n/a
determined, again, through Triclosan n/a 0.3
Water (Aqua) 60.0 60.0
c
Kosmoscience Ciência & Total: 100.0 100.0
Tecnologia Cosmética Ltda,
Brazil.

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | 57

CT2003_Formulating_Genrich_fcx.indd 57 3/20/20 2:22 PM

 Mind Your Microbes

cidal action. A control for residual aluminum
in the armpits also was performed, and only
those without residual aluminum took part in
the study.
The study was carried out by applying a con-
trolled amount of the investigated product (0.5
g) in one of the armpits by spraying after con-
trolled washing. After application, the subjects
were instructed not to wet, wash or pass any
underarm product for the next 48 hr and to not
remove the white cotton shirt provided until the
final evaluation of axillary odor was assessed.
Human axillary microbiome model: Finally,
as noted, a human axillary ex vivo microbiome
model was developed and validated by the
authors’ company. Based on fresh human sweat
from eight healthy subjects, ages 39 to 64 years
(mean age 55 ± 9), the pre-sampled sweat was
pooled, aliquoted and mixed with the respective
test substance (deodorant active). Afterward,
the samples were assayed at 0 hr and 24 hr after
being incubated under controlled conditions
at 37°C. Microbial analyses was carried out in
two ways:

Figure 1. Clinical deodorant efficacy, 24 hr

Figure 2. Clinical deodorant efficacy, 48 hr (a) and percentage of body odor

reduction (b)

58 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2003_Formulating_Genrich_fcx.indd 58 3/20/20 2:22 PM

 Lasting deodorant performance for up to
48 hr was demonstrated for
2-methyl 5-cyclohexylpentanol.
1. Microbial load; i.e., aerobic and anaerobic
colony forming units (CFU). Here, petri dishes
containing plate count agar were aerobically
inoculated with 100 µL of diluted sweat samples
and incubated for 48 hr at 37°C under either
aerobic or anaerobic conditions. The number of
bacterial colonies was assayed and the means of
at least two technical replicates were calculated.
2. Microbiome composition; i.e., bacterial
amplicon sequencing (16S rRNA gene). The
sequencing and bioinformatical evaluation
was performed by a third partyd, wherein
DNA was isolatede and PCR was performed
on variable regions 3 and 4 of 16S rRNA gene.
Sequencing was performed with a reagent kitf
d
CeMeT GmbH, Tübingen, Germany
e
Qiagen MagAttract PowerSoil DNA Kit
f
MiSeq Reagent Kit v3 (600 cycles)
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2003_Formulating_Genrich_fcx.indd 59
and quality of run was 83.05%. The resulting
data was compared with the NCBI Bacterial
16S rRNA database and ordered according
to presence of genus information. The 20
most abundant genera—adding up to 99.4%
of all detected amplicon sequence variants
(ASVs)—were selected based on total abundance
in all experiments and visualized by their
relative abundance.
Results: 24-hr
Deodorant Efficacy
Results from the 24-hr clinical studies of
deodorant efficacy are shown in Figure 1.
According to the expert graders, the triclosan
product showed a significant reduction (p <
0.05) in body odor at 6 hr and 24 hr after single
and multiple applications, in comparison with
| 59
3/20/20 2:22 PM
 Mind Your Microbes

initial values. The same effect was observed at 6 hr

with the test product containing 2-methyl 5-cyclo-
hexylpentanol; however, at 24 hr after regular
application, no significant difference was noted in
comparison to the initial value.
In self-assessments, a significant difference
was reported by the subjects for the 6-hr value
after multiple applications for both test products,
and for the 24-hr value of the test product using
triclosan in comparison to the initial value. For the
comparison of products with each other, no signifi-
cant differences in body odor were documented.

Results: 48-hr
Deodorant Efficacy
Figure 2 shows the results of the 48-hr study.
For the 2-methyl 5-cyclohexylpentanol product,
axillary malodor was reduced by 51.2% 6 hr after
application; 47.9% after 24 hr; and 45.8% after 48
hr. The product therefore achieved a statistically
significant reduction (p < 0.05) in axillary malodor,
compared with untreated armpits at 6 hr, 24 hr and
48 hr. In fact, all participants showed a reduction

Figure 3. Microbial cell count

60 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2003_Formulating_Genrich_fcx.indd 60 3/20/20 2:23 PM

 in axillary malodor for all three time points. In summary, the authors observed viable
The strongest effect was found 6 hr after cell numbers, without differentiation of strain
application. abundance, were significantly reduced when
samples were treated with triclosan—a known,
Results: Human Axillary strong antimicrobial—but remained at compa-
Microbiome Model rable levels to untreated samples when treated
with 2-methyl 5-cyclohexylpentanol.
Microbial load: In the untreated sweat
Microbiome composition: Having explored
samples, a cell count (CFU/mL) of 107 microor-
the abundance of viable microorganisms as
ganisms was detected (see Figure 3), notably
a first step, the next step was to explore the
with an even distribution between aerobic and
relative abundance of different strains. This was
anaerobic microorganisms. Untreated sweat
carried by bacterial amplicon sequencing on a
samples were incubated under controlled
16S rRNA gene level (see Figure 4).
conditions at 37°C (body temperature) and
Untreated sweat samples containing the ini-
proliferated to a level of 108 CFU/mL in slight
tial (0 hr) untreated microbiome were analyzed
favor of the aerobic cells was observed. Sweat
and found to be dominated by Gram-positive
samples incubated under the same conditions
bacteria, mainly consisting of the three genera:
but treated with 0.1% triclosan resulted in
a significant drop of viable cells, compared
with the untreated 24-hr samples, showing
that viability of cells is negatively impacted. Biofilms and the
In comparison, at 24 hr, the cell count for Skin Microbiome
samples treated with 0.1% 2-methyl 5-cyclo-
hexylpentanol were almost identical to those of Check out Page 30 in the
January 2020 digital magazine.
the untreated sample.

Figure 4. Microbiome composition

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | 61

CT2003_Formulating_Genrich_fcx.indd 61 3/20/20 2:23 PM

 Mind Your Microbes
Staphylococcus, Anaerococcus and Corynebacte-
rium. Subsequent incubation of the untreated
sweat samples at 37°C (simulated body tem-
perature) for 24 hr resulted in a slight change in
relative abundance. The amounts of Anaerococ-
cus spp. and Peptoniphilus spp. increased, the
proportion of Corynebacterium spp. remained
almost unchanged, and the relative amount of
Staphylocooccus spp. decreased.
While the 24-hr value for samples treated
with 0.1% of 2-methyl 5-cyclohexylpentanol
was similar to those left untreated, the samples
treated with 0.1% of triclosan showed a
significant enrichment of the Gram-negative
Pseudomonas genus. In combination with the
results shown for the bacterial cell count (Fig-
ure 3), this clearly indicated a selection pressure
toward triclosan-resistant species, resulting in a
severe shift in the axillary microbiome.
Thus, this analysis of the relative microbi-
ome composition revealed that triclosan had
a significant impact on the composition of the
microbiome and caused a significant shift in
abundance. 2-Methyl 5-cyclohexylpentanol, on
the other hand, has very little influence and did
not significantly imbalance the composition of
the microbiome.
Discussion
The two clinical studies discussed reveal two
findings. First, the 24-hr study showed compa-
rable deodorant efficacy of the two ingredients,
triclosan and 2-methyl 5-cyclohexylpentanol.
Both correspond to a significant reduction in
body odor compared with the initial value.
Second, in the 48-hr study, the application of
2-methyl 5-cyclohexylpentanol dramatically
reduced body odor, compared with untreated
armpits at all time points.
Thus, in terms of clinical efficacy, both
modern and conventional systems perform
equally well to reduce malodor, while lasting
performance for up to 48 hr also was dem-
onstrated for 2-methyl 5-cyclohexylpentanol.
Yet, while modern and conventional systems
performed similarly on a sensory level, there
were significant differences on the microbiome
level. The modern system, 2-methyl-5-cyclohex-
ylpentanol, appeared to be more advantageous
in terms of minimally impacting the natural
axillary microbiome. As previously reported,12
it appears unnecessary to indiscriminately
kill all bacteria in order to achieve deodorant
62 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2003_Formulating_Genrich_fcx.indd 62
efficacy, and the present authors hypothesize
that 2-methyl 5-cyclohexylpentanol inhibits
microorganisms, in turn moderating the
development of malodors. The results therefore
suggest that 2-methyl 5-cyclohexylpentanol is a
microbiome-friendly alternative to conventional
organohalogen systems.
Conclusion
Modern cosmetic formulations claiming
lasting deodorant efficacy can benefit from
the proven performance of modern deodorant
actives such as 2-methyl 5-cyclohexylpentanol,
in turn omitting the need for strong antimicro-
bials such as triclosan. This modern alternative
allows formulators to create microbiome-gentle
products without compromising on efficacy.
References
1. Natsch, A. (2015). What makes us smell: The biochemistry
of body odor and the design of new deodorant ingredients,
CHIMIA 69, 414-420.
2. Content Marketing Institute (CMI). (2020). Cosmetic ingredi-
ents consumer database. Symrise AG subscription.
3. Symrise AG. (2019, Nov 11). Farnesol; Nature-identical ses-
quiterpene alcohol. https://www.symselect.com/deodorants
4. Niendorf, H. (2012, Sept). Natural deodorizing active for
modern formulations. Personal Care Magazine, 39-42.
5. Symrise AG. (2019, Oct 11). SymDeo B125; Patented highly
effective deodorant active. https://www.symselect.com/
deodorants
6. Pesaro, M., Diesing, B., Schmaus, G. and Pillai, R. (2011,
Dec). 2-Methyl 5-cyclohexylpentanol: Development of a
novel deodorant agent. SOFW Journal, 137 61-68.
7. Kuhn, W., Wöhrle, I., Dilk, I., Ewering, Ch., Mampel, J.,
Krohn, M. and Zinke, H. (2009, Apr 28). EP2424829 B1,
US8623340B2, BRPI0924661B1….Omega-Cyclohex-
ylalkan-1-oles and use thereof as antimicrobial actives
to combat body odor. http://www.freepatentsonline.
com/8623340.html
8. U.S. National Institutes of Health. (2019, Oct 11). Human
Microbiome Project. https://hmpdacc.org/
9. The Human Microbiome Project Consortium. (2012). Nature
486, (7402) 207-214 and 215-221.
10. Nordzieke, S., Diesing, B., ... Koch, C., et al. (2019). The
good, the bad and the smelly–Developing a representa-
tive model for the human axillary microbiome. Annual
Conference of the Association for General and Applied
Microbiology, poster, Mainz, Germany.
11. Nordzieke, S., Diesing, B., ... Koch, C., et al. (2019). Going
ex vivo–Applying a representative model for the human
axillary microbiome. 25th IFSCC Conference on Cosmetic
Science and Conscience, poster, Milan, Italy.
12. Haustein, U.-F., Herrmann, J., Hoppe, U., Engel, W. and
Sauermann, G. (1993). Growth inhibition of coryneform
bacteria by a mixture of three natural products. Farnesol,
glyceryl monolaurate and phenoxyethanol. HGQ. J Soc
Cosmet Chem, 44 211-220.
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 Formulating | C&T ®

KEY POINTS
• This article reviews the key components
of mascara formulations, including
waxes, film-formers, fillers—and
importantly, packaging.

• Test formulations are created here using

a combined strategy for ingredient
selection and assembly, and assessed for
various properties.

Peer-reviewed

Eye
Formulating Forum

Opener
Combined Formulation Strategy Ensures Mascara Success

Miriam Deola, Marta Montoli

and Nicola Lionetti
Rigano Laboratories S.r.l., Milan

Cecilia Pavesi
University of Milan, Milan

Luigi Rigano, Ph.D.

Institute of Skin and Product
Evaluation (ISPE, S.r.l.), Milan
C onsumer expectations facing mascara
performance and the increasing complex-
ity of formulations has led to continuous
requests for developing innovative recipes,
new brushes and wipers. All the desired
factors cannot always coexist in one for-
mula; it is difficult to simultaneously combine aesthetic targets such
as length, curl, volume and high lash definition. In fact, when trying
to increase the eyelash volume by applying mascara, the increased
weight of the eyelashes results in a reduction in their curl.1

Reproduction in English or any other language of

64 | www.CosmeticsandToiletries.com all or part of this article is strictly prohibited. Vol. 135, No. 4 | April 2020
© 2020 Allured Business Media.

CT2004_Formulating_Lionetti_fcx.indd 64 3/25/20 2:25 PM

 In addition, other important
mascara requirements must be
considered and tested, i.e.: safety
for the eyes and surrounding
skin; easy and even application
without stickiness among the
eyelashes or clumps; fast-drying,
long-lasting wear; and resistance
to flaking, smudging, water and
transfer—but at the same time,
easy and fast removal at the
end of the day. The drying time
must be slow enough for an even
application but not excessively
long, to make the applied film
reasonably permanent.2
A close connection between
a well-performing formula and
the proper applicator can create
a successful mascara. Today,
packaging is a real source of
innovation. It is not only an
attractive, even luxurious, casing
for the formula, but it is also
responsible for the product’s
application function. New
brush materials and shapes,
combinations of fibers created
by 3D printing, and advanced
battery-operated technologies
are launched continuously on
the market.3
Packaging aside, however,
what innovations have occurred
in recent mascara formulation?
In general, the base structure
of formulas has not changed
much in years, although new
raw materials have been made
available to cosmetic formulators.
This article reviews the compo-
nents of mascara formulations
and considers the properties
they impart. In addition, base formulas were
developed and tested using varying ingredients
to determine different product outcomes. The
authors conclude that a combined strategy to
select and assemble ingredients is crucial to
developing a successful mascara.
Mascara Formulating
An overall analysis of global product com-
positions shows a prevalence for oil-in-water
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Formulating_Lionetti_irv.indd 65
A close connection
between a well-
performing formula
and the proper
applicator can create
a successful mascara.
(o/w) anionic emulsions or anhydrous lipid
gels. These are preferred when water resistance
is required. They are composed of pigments
suspended in hydrocarbon solvents, gelled by
organo-modified clays and waxes, and upon
evaporation of the solvent, the waxes act as
plastic film formers.
O/W emulsions are generally based on
anionic emulsifiers; the oil-wax phase, generally
ranging from 25% to 35% may contain stearic/
palmitic/isostearic/oleic acids, which react with
an alkali dissolved in the aqueous phase and
form the corresponding soaps. Thanks to the
successive reaction of soaps with the carbon
dioxide of air, a fatty acid layer forms on the
eyelashes in combination with waxes and film-
forming polymers, creating an insoluble and
flexible film.
Additional emulsifiers with high HLB
values are sometimes used, such as potassium
cetyl phosphate, polyglyceryl-3 methylglucose
distearate or steareth-20/21. The pigments
Elevating
Mascaras
Check out Page 60 in the
March 2019 digital magazine.
L’Oréal Voluminous was the leading mascara
brand in 2019, with US $77.4 million in sales,
followed by L’Oréal Voluminous Lash Paradise,
at $73.3 million.
Source: Statista
| 65
3/18/20 2:16 PM
 Eye Opener
in the formula, at a typical concentration
of around 10-12%, are carbon black or iron
oxides (mainly black), in uncoated form or
coated with alumina and stearic acid, silicones,
polymers, cellulose, lecithin or amino acids.4
Further functional components are humectants,
suspending and chelating agents, preservatives
and specific “active” ingredients for lash-
strengthening and other marketable benefits
marketed to consumers.
Materials and Methods
To explore the influence of key ingredients
and an assembly strategy to optimize mascara
Formula 1. Mascara Base Formula
Phase Ingredients % w/w
A. Water/Aqua qs to 100.0
Disodium EDTA 0.1
Panthenol 0.5
Glycerin 1.0
B. Acacia Senegal Gum 3.5
Hydroxyethylcellulose
C. Triethanolamine 2.5
D. Paraffin 14.0
Copernicia Cerifera Cera
Cera Alba
Euphorbia Cerifera Cera
Steric Acid 3.0
Limnanthes Alba Seed Oil 2.5
Butyrospermum Parkii Butter Extract
E. CI 77499 12.0
F. Antioxidant, Preservatives qs
66 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Formulating_Lionetti_irv.indd 66
properties, a wide systematic study of o/w
mascara emulsions was carried out. The core
ingredient categories assessed included waxes,
film-forming polymers and fillers.
Waxes give body and structure to the
formula. In mascaras, waxes function to
create a thick film on the eyelashes to obtain a
volume-enhancing effect. Waxes also exert other
properties such as lash lengthening, volume
enhancing and curling.
Film-forming polymers create a uniform
film on the surface once a cosmetic product has
been applied, giving long-lasting wear, non-
transfer effects and water resistance. Polymeric
chains arrange in a uniform layer, when
conveyed through a medium that is capable
of evaporating, creating flexible and versatile
films on the eyelashes. Polyurethanes and
polyacrylates are the most used polymers in the
cosmetic field.5
Fillers are inorganic or organic solids that
are insoluble in the vehicle and have different
shapes—i.e., sphere, cube, plate, flake, fiber,
irregular, etc.—and particle sizes, ranging from
nanometers to millimeters. Fillers provide dif-
ferent optical properties, such as transparency
or opacity,6 and absorption performances. In
makeup, they are added for many reasons: to
give volume; influence spreadability and drying
time; modify feel, e.g., softness and velvety/silky
touch; and provide soft-focus effects, water
absorption properties, skin adhesion, transpar-
ency or opacity.7
Test formulas: The pigmented o/w emulsion
used as a base formula for the following trials
is reported in Formula 1. This formulation was
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 Eye Opener

developed taking into consideration some of the was cooled to 40°C while mixing and F, i.e., the
most recurring ingredients used in mascaras on antioxidant and preservatives, were added by
the market. homogenizing. The blend was then cooled further
Formulation procedure: In the main to 25-30°C by slowly mixing for at least 10 min to
container, A was dissolved in water by mixing. allow the emulsion to settle. Complete formula
Ingredients in B were sequentially dispersed stabilization is reached after 24 hr, thus all trials
into A and homogenized with a turbo-emulsifier and evaluations were carried out after 24 hr.
first at RT, then at 65-70°C. Ingredient C was
added by mixing as well. Phases ABC and D Ingredient Variables
were separately heated to 85°C, then D was As noted, several waxes, film-forming poly-
added slowly to ABC by homogenizing with mers and fillers were added to the base formula
turbo-emulsifier for at least 10 min. The to evaluate their influence on technical and
temperature was decreased to ~70°C and E was application characteristics. Ingredients were
added to ABCD in small amounts while homog- selected by considering their recurrence in the
enizing with turbo-emulsifier. The formula market, and application and/or the performance
in mascaras as claimed by raw
material suppliers.
Table 1. Waxes and Waxy Materials Selected Waxes: In the base formula,
the wax content is 14%. For
each trial, half of this amount
Melting (7%) was substituted by one of
Type of wax Key properties
point (°C) 10 different waxes of vegetal or
Vegetal origin; soft; dark olive synthetic origin (see Table 1).
Camellia Sinensis Leaf Film-formers: Nine
60-66 colored with tea scent; good oil-
Wax (Tea Wax)
binding capacity selected film-forming polymers
Jasminum Vegetal origin; soft; amber colored belonging to the acrylate and
Grandiflorum Flower 56-61 with jasmine scent; excellent polyurethane families were
Wax (Jasmine Wax) pay-off tested at 4% active matter in
Helianthus Annuus Vegetal origin; nonpolar; hard; the base formula, as listed in
Seed Wax (Sunflower 74-80 glossy; good oil-binding capacity; Table 2 on Page DM19. In
Wax) pale yellow color the second phase of the study,
Rhus Succedanea Vegetal origin; soft; improves the best-performing waxes
48-54 and polymers were coupled to
Fruit Wax (Sumac wax) lubricity; pale yellow color
Myrica Cerifera Fruit Vegetal origin; quite hard; obtain model formulas through
45-55 balanced-fit combinations for
Wax (Myrica Fruit Wax) spreadable; pale yellow colored
the best possible synergies.
Mixture (A): Helianthus
Annuus Seed Wax, Fillers: At this stage, in order
Vegetal origin; quite hard; flexible; to optimize mascara applica-
Shorea Robusta Resin, 72-78
pale yellow color tion and performance, seven
Rhus Succedanea
Fruit Wax fillers were tested at 6% since
Animal origin (excretion product of at higher loads, they can form
Kerria Lacca); very hydrophobic; lumps. Exceptions included the
Shellac Cera 78-84
adhesive; volumizing; yellow to
amber color
Tetradecyloctadecyl Synthetic origin; hard and brittle;
33-38
Stearate white color
Synthetic origin; rigid and
Cetearyl Behenate 60-65 structuring; white to light yellow
color
Mixture (B): Cera Alba,
Natural/synthetic origin; elastic;
Ceteareth-25, Oryza 60-66
off-white color
Sativa Bran Cera

68 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Formulating_Lionetti_fcx.indd 68 3/25/20 11:59 AM

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Table 2. Polymers Selected for Trials

Polymer Appearance Solid % Properties

Length and volume,
Styrene/Acrylates Copolymer, Aqua Milky white fluid 48
water-resistance
Styrene/Acrylates/Ammonium Volume, water and
White emulsion 41
Methacrylate Copolymer, Aqua transfer resistance
Ethylene/Acrylic Acid Copolymer,
White emulsion 30 Curl, high gloss, definition
Styrene/Acrylates Copolymer, Aqua
Acrylates/Ethylhexyl Acrylate Copolymer,
Long lasting, adhesion,
Acrylates/ Dimethylamino-ethyl White emulsion 40
flexibility, high gloss
Methacrylate Copolymer, Aqua
Length, water and
Acrylates Copolymer, Aqua White emulsion 41
transfer resistance, gloss
Isododecane, Dimethicone, Viscous, slightly Long lasting,
20
Polyethacrylate hazy liquid water resistance, flexibility
Acrylates/Ethylhexyl Acrylate Copolymer, Milky white Adhesion, water and
48
Aqua, Aminomethyl Propanol emulsion rub resistance, gloss
Length and volume,
Polyurethane-A, Aqua White emulsion 40
definition
Length and volume,
Polyurethane-B, Aqua White emulsion 40
adhesion

Table 3. Fillers Used for Trials

Filler Particle size Properties

Nano-sized particles with a specific surface area of
Silica 12 nm
200 m2/g, thickening and texturizing
Talc 40 μm Plate-shaped particles, texturizing, transparency
Kaolin 0.4 μm Plate-shaped particles, oil absorption, adhesion, soft touch
Polyamide-5 8-12 μm Adhesion, curling effect, shorter drying time
Spherical glass particles, high transparency, optical effects,
Glass beads 40 μm
texturizing
PEG-15/PPG-70 Glyceryl
Urethane powder with a ball-bearing effect, oil-absorption,
Ether/IPDI/DMPA Cross- 5-8 μm
soft-focus, slip, coverage
polymer
Solid spheres with smooth surface, mattifying, oil-
Polymethyl Methacrylate 5-15 μm
absorption

DM19 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Formulating_Lionetti_irv.indd 70 3/18/20 2:17 PM

 Mascara removal was considered ‘easy’
for all formulas and comparable to the
base formula.
thickener silica at 2% since it affects viscosity;
and the glass beads at 3%. The filler powders
selected are shown in Table 3.
Test Protocol
The resulting formulas were analyzed from a
technical and application/sensorial point of view.
pH was measured at 25°C with pH metera; vis-
cosity measurements were carried out 24 hr after
preparation at 25°C with a rotational viscom-
eterb; and each sample was centrifugedc at 37°C
and 7090 G for 30 min, 24 hr after preparation.
Drying time: The drying time was tested by
applying a layer of mascara on false eyelashes
with the same brush for all the products. After
a
S20 SevenEasy, Mettler-Toledo AG
b
Brookfield RVT, Helipath T-E/F, 2.5-5-10 rpm
c
Multifuge 1S-R Heraeus
a)
c)
Figure 1. Brushes used for test applications; the first set of tests used brush A; later
applications used brushes B-D.
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Formulating_Lionetti_irv.indd 71
2 min and 5 min, the eyelashes were dragged
across a white sheet of paper to observe the
imprint left behind, indicating the product’s
transferred amount.
Water resistance: Water resistance was eval-
uated only for the polymer-containing formulas
by applying a small amount of product (0.06 g)
on a limited area of the volar forearm (4 cm ×
2 cm). After 30 min, the forearm was wetted
with a jet of tap water and the area was rubbed
by hand 10 times under consistent pressure and
force. Each product was compared with the
base formula (without polymer) by conducting
this test on five subjects.
Application properties: Application proper-
ties were evaluated by a panel of 10 expert
users, i.e., 25-50 year-old women who use
cosmetics, according to the following param-
eters: ease of application, lash separation,
b)
d)
| DM20
3/18/20 2:17 PM
 Eye Opener

lengthening-volumizing-curling
effects, easy removal and residue
after removal. The volunteers
scored the samples on a scale of
1-10 for each parameter, blindly
evaluating the base formula
(standard) versus a test formula
with the additive.
Brushes: For all preliminary
tests, the same silicone brush
was used, characterized by short
and well-spaced bristles, which
allows for an easily spreadable
application (see Figure 1, brush
A). The test formulas obtained
by the combination of additives
were applied with a series of
brushes, each comprising differ-
ent materials, designs and bristle
length (see Figure 1, brushes B,
C and D).

Waxes: Results and

Discussion
Table 4. Viscosity Data for Different Waxes The pH values measured for
all formulas were within the
range of 8.3-8.7. Viscosity values
Viscosity (25°C)b 2.5 rpm 5 rpm 10 rpm are reported in Table 4; these
were slightly lower for all the
Base formula 640,000 375,000 230,000
substituting waxes in comparison
Camellia Sinensis Leaf Wax with the base formula—in par-
560,000 340,000 190,000
(Tea Wax)
ticular, for mixture B (very low
Jasminum Grandiflorum viscosity) and except for sumac
500,000 300,000 175,000
Flower Wax (Jasmine Wax) wax, whose viscosity was higher.
Helianthus Annuus Seed It was also noted that none of
560,000 350,000 195,000
Wax (Sunflower Wax) the centrifuged samples showed
Rhus Succedanea Fruit Wax signs of separation.
760,000 450,000 235,000
(Sumac Wax) Drying times: As far as drying
Myrica Cerifera Fruit Wax times, the base formula dried
580,000 360,000 200,000
(Myrica Fruit Wax) more slowly in comparison
Mixture (A): Helianthus with the formulas containing
Annuus Seed Wax, Shorea sunflower wax, myrica fruit wax,
540,000 330,000 205,000
Robusta Resin, Rhus shellac wax, tetradecyloctadecyl
Succedanea Fruit Wax stearate, cetearyl behenate and
Shellac Cera 580,000 370,000 220,000 sumac wax. The drying time
Tetradecyloctadecyl Stearate 500,000 350,000 185,000 was similar between the base
formula and those containing tea
Cetearyl Behenate 520,000 300,000 180,000
wax, jasmine wax and mixture
Mixture (B): Cera Alba, A. Mixture B showed a rather
Ceteareth-25, Oryza Sativa 140,000 110,000 65,000 longer drying time. Examples at
Bran Cera
2 min and 5 min of the imprints
table footnote: at t = 24 hr for each mascara
left by the base, sunflower wax
and mixture B formulas applied

DM21 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Formulating_Lionetti_irv.indd 72 3/18/20 2:17 PM

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to test eyelashes are shown in Figure 2a-c. Polymers:

Application properties: In Table 5 and
Figure 3, the average scores (with standard
Results and Discussion
deviations) given by the panelists for each The pH values for all formulas fell within the
formula for the five parameters are reported. range 8.4-8.7; their viscosity values are reported
The base formula was considered as a standard in Table 6. The addition of polymers gave rise
for comparison, with an average score of six for to increased viscosity values. Nevertheless, this
each parameter. Mascara removal was consid- does not represent a limit for the application of
ered “easy” for all formulas and comparable to mascaras on the lashes.
the base formula. The waxes that showed better Once again, none of the centrifuged samples
performance when added to the base mascara showed signs of separation. The drying time of
were tea, jasmine, sunflower, sumac, myrica the base formula was shortened by the addition
fruit, shellac wax and mixture A. These waxes of polymers. This was evaluated by means of
were subsequently combined with the best- the drying test with false eyelashes and was
performing polymers and fillers to obtain new perceived by the panelists during application
finished test formulas. trials. Examples of the imprints after 2 min
and 5 min left by the
base, styrene/acry-
lates copolymer and
acrylates/ethylhexyl
a) b) c) acrylate copolymer
formulas are shown
in Figure 4a-c.
Water resistance:
Water resistance tests
showed different
results depending on
the polymer used in a
formula. For polyure-
thanes, no significant
improvements were
noted in terms of
washing resistance
in comparison with
the base formula,
as well as for other
polymers: acrylates
Figure 2. Drying time test imprints after 2 min (above) and 5 min copolymer; ethylene/
(below) of: base (a), sunflower wax (b) and mixture B (c) formulas acrylic acid copo-
lymer and styrene/

Table 5. Average Scores for Application Properties with Different Waxes

Parameter Tea Jasmine Sunflower Sumac Myrica Shellac Mixture A

Ease of application 6.4 ± 0.8 6.3 ± 0.8 8.5 ± 1.1 5.3 ± 1.4 8.5 ± 0.8 5.8 ± 1.0 6.3 ± 0.8
Eyelash separation 8.3 ± 0.9 7.5 ± 0.8 7.3 ± 0.7 6.1 ± 1.3 8.3 ± 0.9 6.7 ± 0.9 8.3 ± 0.9
Lengthening effect 8.4 ± 1.0 7.6 ± 1.1 7.4 ± 1.0 6.2 ± 1.0 7.6 ± 0.7 7.0 ± 0.9 7.3 ± 0.9
Volumizing effect 7.4 ± 1.0 7.4 ± 0.8 6.7 ± 1.3 7.1 ± 0.9 7.3 ± 0.9 6.2 ± 1.2 7.2 ± 0.8
Curling effect 6.5 ± 0.8 6.4 ± 0.7 7.3 ± 1.3 6.1 ± 1.1 6.5 ± 0.8 6.2 ± 1.1 6.5 ± 0.8

DM23 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Formulating_Lionetti_irv.indd 74 3/18/20 2:17 PM

 acrylates copolymer; sty-
rene/acrylates/ammonium
methacrylate copolymer; and
styrene/acrylates copolymer.
Polymers showing enhanced
water resistance were:
acrylates/ethylhexyl acrylate
copolymer and acrylates/
dimethylaminoethyl methac-
rylate copolymer; acrylates/
ethylhexyl acrylate copoly-
mer; and polyethacrylate.
Application benefits: The
application benefits provided
by polymers are reported
in Table 7; average scores
were tallied (with standard
deviation) for parameters
including: eyelash separa- Figure 3. Average scores of application properties with
tion, lengthening effect, different waxes
volumizing effect and curling
effect. The base formula
was considered the standard
for comparison, and again, Table 6. Viscosity Data with Different Polymers
scored an average of six for
each parameter.
The application was
Viscosity (25°C)b 2.5 rpm 5 rpm 10 rpm
considered similar to the Base formula 640,000 375,000 230,000
base formula for all the Styrene/Acrylates Copolymer,
860,000 500,000 285,000
references, and was rated Aqua
as easier to apply in the Styrene/Acrylates/Ammonium
case of polyethacrylate and 1,260,000 680,000 375,000
Methacrylate Copolymer, Aqua
acrylates/ethylhexyl acrylate Ethylene/Acrylic Acid Copolymer,
copolymer. Acrylates/ethyl- Styrene/Acrylates Copolymer, 1,140,000 670,000 370,000
hexyl acrylate copolymer and Aqua
its mixture with acrylates/ Acrylates/Ethylhexyl Acrylate
dimethylaminoethyl meth- Copolymer, Acrylates/
1,360,000 830,000 445,000
acrylate copolymer are not Dimethylaminoethyl Methacrylate
reported because while they Copolymer, Aqua
had a positive influence on Acrylates Copolymer, Aqua 1,100,000 610,000 350,000
eyelash separation and long
Isododecane,
lasting effects, their length- Dimethicone, 770,000 440,000 250,000
ening/curling/volumizing Polyethacrylate
performances did not show a Acrylates/Ethylhexyl
significant enhancement. Acrylate Copolymer,
Mascara removal was 840,000 490,000 265,000
Aqua, Aminomethyl
considered easy for all the Propanol
formulas except for acry- Polyurethane-A, Aqua 1,100,000 620,000 365,000
lates/ethylhexyl acrylate
Polyurethane-B, Aqua 970,000 550,000 310,000
copolymer and its mixture
with acrylates/dimethyl-
table footnote: at t = 24 hr for each mascara
aminoethyl methacrylate
copolymer, polyethacrylate,

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | DM24

CT2004_Formulating_Lionetti_irv.indd 75 3/18/20 2:17 PM

 Eye Opener

styrene/acrylates/ammonium methacrylate Results: Polymer and

copolymer. These results are shown in Figure 5.
As shown here, all polymers provided
various benefits to the base formula except
polyurethane-A, which performed slightly less
effectively than the others. The best polymers selected by taking into consideration several
were then associated with the selected waxes to criteria compensating for the advantages and
obtain finished formulas.
a) b) c)
Figure 4. Drying time test imprints after 2 min (above) and
5 min (below) of: base (a), styrene/acrylates copolymer (b)
and acrylates/ethylhexyl acrylate copolymer (c)
Wax Combinations
Plus Fillers
Combinations of polymers and waxes were
limitations of the two ingredients, which were
associated by mutual combination. As
an example, tea wax was associated
with acrylates copolymer. This wax
is soft and provides lengthening and
volumizing effects, together with ease
of application. The polymer counteracts
the slow drying time and lower viscosity
of the formula containing only tea wax,
and provides a curling effect besides
boosting length and volume.
Another formula was prepared
combining sunflower wax and styrene/
acrylates copolymer. This wax provides
beneficial application properties such
as length and curl. The polymer fills the
gap for eyelash separation and volume
properties. In this case, the wax also
compliments the polymer in terms of
viscosity and drying time.
At this stage, the fillers were tested
in order to further optimize the applica-
tion and performance properties of the
test formulas. The addition of fillers

Table 7. Average Scores for Application Properties with Different Polymers

Ethylene/
Styrene/
Acrylic Acid
Styrene/ Acrylates/
Acrylates Copolymer Polyeth-
Parameter Acrylates Polyurethane-A Ammonium Polyurethane-B
Copolymer and Styrene/ acrylate
Copolymer Methacrylate
Acrylates
Copolymer
Copolymer
Eyelash
8.5 ± 0.8 6.4 ± 1.0 7.5 ± 0.8 7.2 ± 1.1 8.7 ± 1.1 8.4 ± 1.0 5.4 ± 1.4
separation
Lengthening
8.8 ± 1.0 7.5 ± 1.0 8.7 ± 1.2 8.7 ± 0.9 8.6 ± 0.8 7.0 ± 0.9 8.5 ± 1.1
effect
Volumizing
7.9 ± 0.7 7.4 ± 0.8 7.5 ± 1.1 9.1 ± 0.9 6.6 ± 0.8 6.2 ± 1.2 9.2 ± 0.8
effect
Curling effect 7.6 ± 1.0 6.4 ± 1.0 7.4 ± 1.1 9.0 ± 1.1 6.2 ± 1.1 7.1 ± 1.2 7.2 ± 0.8
Curling effect 6.5 ± 0.8 6.4 ± 0.7 7.3 ± 1.3 6.1 ± 1.1 6.5 ± 0.8 6.2 ± 1.1 6.5 ± 0.8

DM25 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Formulating_Lionetti_irv.indd 76 3/18/20 2:17 PM

 increased the viscosity of the formula, while the
pH values remained stable (pH 8.4-8.6). Samples Elevating
subjected to the centrifuge test once again did not Mascaras
show any sign of separation.
The results of the panel evaluation after the Click to Page 60 in the
addition of fillers to the formula with tea wax and March 2019 digital magazine.

acrylates copolymer are

reported in Table 8.
The base formula with
tea wax at 7% and the
polymer at 4% a.m.
was given a score of
six for all the param-
eters and served as
the comparison.
Figure 6 shows the
average scores of the
best fillers represented
by means of a radar or
spider graph. In this par-
ticular formula, talc and
PEG-15/PPG-70 glyceryl
ether/IPDI/DMPA cross-
polymer did not prove to
perform sufficiently in
any of the parameters.
Based on the
obtained results, to the
formula containing tea
wax and acrylates copo-
Figure 5. Average scores of application properties with
lymer, fillers were added
different polymers

Table 8. Scores for Application of Tea Wax+Acrylates Copolymer with Different Fillers

PEG-15/PPG-70
Polymethyl
Polyamide-5, Glass Glyceryl Ether/
Silica, 2% Talc, 6% Kaolin, 6% Methacrylate,
6% beads, 3% IPDI/DMPA
6%
Crosspolymer, 6%
Ease of
5.3 ± 1.3 6.8 ± 0.6 6.0 ± 1.1 8.2 ± 1.1 6.4 ± 0.8 6.2 ± 1.1 6.3 ± 0.5
application
Eyelash
7.3 ± 1.8 7.1 ± 1.0 6.7 ± 1.3 8.1 ± 1.2 5.6 ± 1.1 7.1 ± 1.4 7.4 ± 1.2
separation
Lengthening
6.2 ± 1.1 6.2 ± 0.8 6.7 ± 1.1 6.7 ± 0.5 5.8 ± 0.8 6.8 ± 1.1 6.2 ± 0.8
effect
Volumizing
8.5 ± 1.0 5.8 ± 0.4 7.8 ± 1.1 6.2 ± 1.0 7.8 ± 1.3 6.1 ± 0.6 8.5 ± 1.1
effect
Curling
5.8 ± 0.8 5.8 ± 0.4 6.0 ± 0.7 6.0 ± 0.7 5.8 ± 0.4 6.2 ± 1.0 6.1 ± 0.6
effect

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | DM26

CT2004_Formulating_Lionetti_irv.indd 77 3/18/20 2:17 PM

 Eye Opener

including: silica, kaolin and glass beads—all of
these are useful to obtain volume and filling.
It was necessary to adjust the use percentage
to avoid an excessive increase in viscosity and
change in drying speed that would negatively
influence the ease of application.
Photographs were taken of the formulas
applied to eyelashes (or not) as follows: without
mascara and with the base formula applied
using brush A (see Figure 7a-b), then with
the final formula applied using brushes B and
D (see Figure 8a-b). As shown here, brush B
emphasized the volume and
thickened the eyelashes.
On the contrary, brush
D enhanced the length
of lashes and improved
their definition.

Conclusions
This study underlines
the advantages of adopting
a combined strategy for
the selection and proper
assembly of ingredients
responsible for mascara
structure. High melting
point waxes must be used
at high percentages in order
to obtain a lengthening
effect via the creation of a
hard and thin film. A low
melting point wax like tea
wax is more suitable for its
Figure 6. Average scores of application properties of tea wax + volume-enhancing effect,
acrylates copolymer mascara with different fillers giving a creamy texture

DM27 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Formulating_Lionetti_irv.indd 78 3/18/20 2:17 PM

 and a thicker
film. Curling a) b)
effects can be
achieved with
the more plastic
waxes, maintain-
ing the shape
of eyelashes.
Film-forming
polymers are
essential to
create a film on Figure 7. Eyelashes without mascara (left) and with base
the eyelashes formula applied using brush A (right)
that boost length,
water resistance
and definition.
In general, poly-
mers accelerate a) b)
the drying time.
This feature can
be exploited
when combin-
ing polymers
with waxes
according to the
described cri-
teria of mutual
compensation
(systematic fit-
Figure 8. Eyelashes with the final formula applied using
ting); i.e., to fill brush B (left) and brush D (right)
the respective
gaps and benefits.
Semi-definitive formulas can be obtained by only with application onto actual eyelashes that
the addition of fillers. These are fundamental for one can truly evaluate whether the formula is
a volume-enhancing effect but the identification adequately performing or not.
of the correct balance among the filler types and
amounts ease application and formula thicken- References
ing—this requires an experience-based approach.
1. Mori A., Takahashi H., Yokoyama H., Tomomasa S., Takahashi
Fillers can exert different functions depending S., Morohoshi F.; Development of a unique and novel mascara
on the physical properties. They can improve using a ‘Balloon Powder’ which has a dual effect on both
ease of application and eyelash separation thanks the volume and the curl of eyelashes; paper, 23rd IFSCC
Congress, Orlando, USA (2004).
to the slip of the fillers. In general, this last
2. Rieger M. M.; Harry’s Cosmeticology; 8th Edition; Chemical
effect is related to an increase in volume of the Publishing, New York, (2000); 564-567.
eyelashes, but avoids the risk of forming lumps 3. Steinbach K.; Innovation between evolution and revolution;
during application. Powders that improve the Household and Personal Care Today n.1 (2012); 7-9.
volume effect can hardly enhance the curl at the 4. Lionetti N., Rigano L.; Zooming in on HD cosmetics: soft focus
effects; Cosmetics & Toiletries Vol. 133 n.3 (2018); 52-63.
same time.
5. Valsesia P., Pirovano C., Crusco C., Hanno I., Vitali A., Saligari
For this type of makeup, the choice of the
F., Bettinelli S., Depta G.; Shape-adapting film formers based
most suitable packaging can dramatically on linear siliconic polyurethanes; paper, 24th IFSCC Confer-
influence the result of application onto the ence, Seoul, Korea (2017)
eyelashes. It also is worth highlighting that the 6. Wypych G.; Handbook of fillers; 2nd edition; ChemTec
Publishing, Toronto, Canada (1999); 3-7.
proper application tests are necessary to assess
7. Rigano L.; Color foundation and base formulas deciphered;
the performance of these cosmetic products. It is
Cosmetics & Toiletries Vol. 127 n.3 (2012); 152-156.

Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries® | DM28

CT2004_Formulating_Lionetti_irv.indd 79 3/18/20 2:17 PM

 Formulating | C&T ®
The following formulas are offered for your
consideration as a basis from which to build
and create your own. The information is listed
as originally provided by suppliers. Readers
should note that in some cases, companies or
ingredients may have changed.
Want More Formulas?
Click to Page DM29 for the expanded formulary,
complete with interactive links to the free
Cosmetics & Toiletries Bench Reference.
Sun Care Formulary
SUNSCREEN CREAM SPF 45
(Acme-Hardesty Co.)
Climate change and global warming have made
sunscreens a part of consumers’ daily wear routines. To
improve sun protection, combining different UV filters
and absorbers is a must, which consequently increases
the oily phase in the end formula. Using high amounts of
non-polar preservatives in the oil phase, however, poses
risks of contamination since low-polar preservatives
tend to migrate into the oily phase, leaving the aqueous
phase unprotected. SharoSense Plus 184 provides
the answer. This innovative polar preservative system
brings uncompromised antimicrobial efficacy at low use
levels (0.7%).
A. Water (aqua) qs to 100.00% w/w
EDTA 0.10
Maltol (and) Didecyldimonium Chloride
(Sharosense Plus 184, Sharon Laboratories Ltd.) 0.70
Xanthan Gum 0.50
B. Caprylic/Capric Triglyceride 5.00
Cetearyl Alcohol (and) Cetearyl Glucoside (Montanov 68,
Seppic) 3.00
PVP/VP/Eicosene Copolymer (Antaron V-220, Ashland LLC) 3.00
Ethylhexyl Methoxycinnamate 7.50
Octyl Salicylate 5.00
Benzophenone-3 6.00
Butyl Methoxydibenzoylmethane 1.60
Homosalate 10.00
Titanium Dioxide 3.00
Tocopheryl Acetate 1.10
Ceteareth-20 (and) Cetearyl Alcohol (Cosmowax BP, J and P, Croda) 3.00
Procedure: Heat water to 45-50°C. Add remaining A in the order listed with mixing,
ensure complete dissolution before adding the next ingredient. Heat B to 50-60°C
while stirring until melted and unified. Homogenize batch at approx. 55°C.
UV ARREST CONTINUOUS SPRAY
(Ashland LLC)
This anhydrous SPF 70 aerosol is very water resistant,
non-tacky and has low shine.
A. SD Alcohol 40 59.00% w/w
VA/Butyl Maleate/Isobornyl Acrylate Copolymer
(Advantage Plus, Ashland LLC) 2.00
70 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Sun_Care_Frmlry_fcx.indd 70
B. Benzophenone-3 (Escalol 567, Ashland LLC) 3.00
Butyl Methoxydibenzoylmethane (Escalol 517, Ashland LLC) 6.00
Octyl Salicylate (Escalol 587, Ashland LLC) 5.00
Octocrylene (Escalol 597, Ashland LLC) 10.00
Homosalate (Neo Heliopan HMS, Symrise AG) 15.00
100.00
Procedure: Combine A until fully dissolved. Separately combine B and heat on low
until crystals are dissolved. Add B to A. Continue mixing until homogenous.
NATURAL BABY GOODNESS SPF 30
(BASF Corp.)
This formulation has been specifically developed for
delicate skin that needs superior protection. Z-Cote
LSA-UC, a large-particle, mineral UV filter forms a
protective layer on the skin to reflect, scatter and absorb
harmful UVA and UVB rays. Cetiol RLF compliments
the formula with its superior sensory attributes.
Both ingredients have passed the National Products
Association (NPA) strict guidelines to further guarantee
consumer confidence.
A. Water (aqua) 44.40% w/w
Glycerin 2.00
Sodium Chloride 0.50
Preservatives 0.10
B. Magnesium Sulfate 1.50
Polyglyceryl-2 Polyhydroxystearate (Dehymuls PGPH,
BASF SE) 3.00
Polyglyceryl-3 Diisostearate (Lameform TGI, BASF SE) 2.00
Titanium Dioxide (and) Coconut Alkanes (and) Stearic
Acid (and) Polyhydroxystearic Acid (and) Alumina (and)
Coco-Caprylate/Caprate (UV Cut TiO2-60-VL,
Grant Industries Inc.) 14.00
Zinc Oxide (Z-Cote LSA-UC, BASF Corporation) 13.40
Caprylyl Caprylate/Caprate (Cetiol RLF, BASF SE) 12.00
Oleyl Erucate (Cetiol J 600, BASF SE) 2.00
Dicaprylyl Ether (Cetiol OE, BASF SE) 5.00
Polyhydroxystearic Acid (Pelemol PHS-8, Phoenix
Chemical Inc.) 0.10
100.00
Procedure: Combine A in main beaker under high prop mix. Combine B in side
beaker. Begin heating under very slow prop mixing, increasing speed as phase
melts. Heat A and B to 75-85°C under high speed prop mix. At 80°C, move B to
homogenizer and mill for 1-2 min. Add milled B to A slowly; when uniform, move
to slow sweep and begin cooling to below 35°C; note: microbial testing has not
been carried out on this formula.
3/18/20 2:39 PM
 who is the safety belt
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we are.

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 EXPANDED Sun Care Formulary
ANTI-AGING FACE CREAM WITH
PUERARIA MIRIFICA
AND SUPERFRUIT
(Bio-Botanica Inc.)
A. Water (aqua) qs to 100.00% w/w
Glycerin 4.00
Glycerin (and) Water (aqua) (and) Pueraria Mirifica Root Extract
(Puresterol, Bio-Botanica Inc.) 3.00
B. Emulsifying Wax NF 9.00
Theobroma Cacao (Cocoa) Seed Butter 5.00
Stearic Acid 3.25
Zea Mays (Corn) Oil 2.50
Caprylic/Capric Triglyceride 2.00
Cetyl Alcohol 2.00
C. Lycium Barbarum (Goji) Fruit Extract (and) Coffea Arabica
(Coffee) Fruit Extract (and) Euterpe Oleracea Fruit Extract
(and) Morinda Citrifolia Fruit Extract (and) Punica Granatum
Extract (and) Garcinia Mangostana Fruit Extract (and)
Camellia Sinensis Leaf Extract (and) Propanediol (Superfruit
Blend, Bio-Botanica Inc.) 0.50
D. Water (aqua) 5.00
Potassium Sorbate 0.40
Sodium Benzoate 0.30
Procedure: In main beaker, mix A with lightening mixer then heat to 60°C. In a sepa-
rate vessel, weigh and heat B to 60°C. Add B to A and mix for 10 min at 60°C.
Separately mix D. Begin cooling main batch under agitation. When batch reaches
40°C, add C to AB, followed by D premix; properties: appearance = heavy beige
cream; pH = 5.5-6.5.
DM29 | www.CosmeticsandToiletries.com Vol. 135
CT2004_Sun_Care_Frmlry_fcx.indd 72
LIGHT TAN LOTION
(Centerchem Inc.)
This sunless tanning lotion has sun protection and
moisturizing properties.
A. Ceteareth-6 (and) Stearyl Alcohol 2.00% w/w
Glyceryl Stearate (Tegin M Pellets, Evonik Industries AG) 1.00
Cetyl Alcohol (Tego Alkanol 16, Evonik Industries AG) 2.00
Dimethicone (DC 200 Fluid, Dow Corning Corp.) 1.00
Cyclopentasiloxane (DC 345 Fluid, Dow Corning Corp.) 1.50
Ethylhexyl Methoxycinnamate (Parsol MCX, DSM
Personal Care) 2.00
Butyl Methoxydibenzoylmethane (Parsol 1789,
DSM Personal Care) 1.00
B. Water (aqua) 60.70
Xanthan Gum 0.30
C. Propylene Glycol 4.00
Phenoxyethanol (and) Ethylhexylglycerin
(euxyl PE 9010, schulke) 0.50
Sodium Hyaluronate 4.00
D. Water (aqua) 5.00
Dihydroxyacetone 3.50
Erythulose (proposed) 1.50
90.00
Procedure: Combine B and mix until uniform. Add C to B. Separately heat A and
BC to 75°C. Add A to BC under moderate mixing. Homogenize briefly. Cool.
Separately combine D and add to batch at 40°C. Mix until uniform. If necessary,
adjust pH of batch to 4.0–4.5. Discontinue batch at 30°C.
W/O MULTI-CULTURAL
UNDER-EYE CONCEALER
SPF 50+ BROAD SPECTRUM
(Croda)
This multi-cultural under-eye concealer with SPF is the
perfect remedy for dark circles. Sensasil PCA assists in
spreadability and delivers a long-lasting, silky after-
feel. The high SPF is achieved by using Solaveil XT-300
in the oil phase, Solaveil XT-40W in the water phase
and SolPerForm 100, which creates even coverage.
Available in a light, medium and dark shade, this
under-eye concealer is suited for any ethnicity.
A. PCA Dimethicone (Sensasil PCA, Croda) 2.00% w/w
PEG-30 Dipolyhydroxystearate (Cithrol DPHS, Croda) 2.00
Ricinus Communis (Castor) Seed Oil 4.00
Hydrogenated Castor Oil 1.00
PPG-15 Stearyl Ether (Arlamol PS15E, Croda) 3.00
B. Titanium Dioxide (and) Caprylic/Capric Triglyceride (and)
Polyhydroxystearic Acid (and) Stearic Acid (and) Alumina
(Solaveil XT-300, Croda) 7.00
Caprylic/Capric Triglyceride (and) Titanium Dioxide (and)
Polyhydroxystearic Acid (and) Aluminum Stearate (and)
Alumina (Solaveil CT-300, Croda Europe Ltd.) 22.00
C. Water (aqua) 30.60
Glycerin 2.00
Hydrolyzed Wheat Protein/PVP Crosspolymer/Water (aqua)
(SolPerForm 100, Croda) 2.00
Titanium Dioxide (and) Water (aqua) (and) Polyglyceryl-2
Caprate (and) Sucrose Stearate (and) Simmondsia
Chinensis (Jojoba) Seed Oil (and) Stearic Acid (and)
Alumina (and) Glyceryl Caprylate (and) Squalane
(Solaveil XT-40W, Croda Europe Ltd.) 4.00
Magnesium Sulfate Hepta-Hydrate 1.00
D. Caprylic/Capric Triglyceride (Crodamol GTCC, Croda) 12.00
CI 77499 (SunPURO Black Iron Oxides, Sun Chemical Corp.) 0.60
(SunPURO Red Iron Oxides, Sun Chemical Corp.) 1.20
CI 77492 (SunPURO Yellow Iron Oxides, Sun Chemical Corp.) 5.00
E. Phenoxyethanol 0.60
100.00
No. 4 | April 2020
3/18/20 2:40 PM

Procedure: Add A to main beaker and heat to 80-85°C until fully melted and uniform
with slow propeller mixing. Combine all of D and pass on the roller mill 3 until the
dispersion is fully dispersed and free of striations (make D @ 150% to account for
loss while processing). In a side beaker, add B and heat to 80-85°C. When A, B
and D are at 80-85°C, combine BD and add to A and start medium speed propel-
ler mixing maintaining temperature at 80-85°C. In another side beaker, add all of C
with propeller mixing and heat to 80-85°C until uniform (adjust speed accordingly
to ensure dispersion). When ABD and C are at their appropriate temperatures
and uniform, pour C into ABD extremely slowly, while high speed propeller mixing
(adjust speed accordingly as batch viscosity will increase as the water phase is
incorporated). After all of C is transferred, continue mixing until uniform and cool
the batch to RT. At 35°C, add E and continue mixing until uniform. At RT, stop
mixing and check specifications.
UV BLOCKING PROTECTOR
(Elementis)
This rich sun cream gives broad UV protection using
inorganic sunscreen filters, with a predicted SPF of 20.
Bentone Luxe WN provides body and stability of the
UV filters, while performing as the only emulsifier in
the system.
A. Dicaprylyl Carbonate 35.90% w/w
Caprylic/Capric Triglyceride (and) Stearalkonium Hectorite
(and) Polyglyceryl-3 Diisostearate (and) Polyglyceryl-3
Polyricinoleate (Bentone Luxe WN, Elementis) 15.00
Fragrance (parfum) 0.10
B. Zinc Oxide (and) Triethoxycaprylylsilane (Z-Cote HP1, BASF
Corporation) 10.00
Titanium Dioxide (and) Silica (and) Dimethicone (Parsol TX ,
DSM Personal Care) 7.50
C. Water (aqua) 30.00
Phenoxyethanol (and) Ethylhexylglycerin (euxyl PE 9010,
schulke) 1.00
Magnesium Sulfate Hepta-Hydrate 0.50
100.00
Procedure: Combine A with stirring until uniform. Add B to A with Silverson, homog-
enizing for 10 min. Combine C and mix until dissolved. Slowly add C to AB with
propeller mixing until uniform.
HIGH SPF SUNSCREEN
WITH US-APPROVED FILTERS
(Evonik Industries AG)
A. Cetyl PEG/PPG-10/1 Dimethicone (Abil EM 180, Evonik
Industries AG) 2.00% w/w
Octocrylene 10.00
Microcrystalline Wax 1.20
Hydrogenated Castor Oil 0.80
Propylene Glycol 0.00
EDTA 0.00
Triisostearin (Tegosoft TIS, Evonik Industries AG) 2.00
Diethylhexyl Carbonate (Tegosoft DEC, Evonik Industries AG) 2.00
Cetyl Dimethicone (Abil Wax 9801, Evonik Industries AG) 2.00
Ethylhexyl Methoxycinnamate 7.50
Ethylhexyl Salicylate 5.00
Homosalate 15.00
Butyl Methoxydibenzoylmethane 3.00
Benzophenone-3 6.00
B. Water (aqua) 40.00
Propylene Glycol 3.00
Sodium Chloride 0.10
EDTA 0.10
C. Propylene Glycol (and) Diazolidinyl Urea (and) Methylparaben
(and) Propylparaben (Germaben II, Ashland LLC) 0.30
D. Fragrance (parfum) qs
100.00
Procedure: Heat A to approx. 80°C. Add B at 80°C or RT slowly while stirring. Ho-
mogenize for a short time. Cool with gentle stirring and add C to AB below 40°C.
Homogenize again below 30°C and add D.
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Sun_Care_Frmlry_fcx.indd 73
EXPANDED Sun Care Formulary
PRE-SUN LOTION
(Floratech)
This pre-sun lotion with mineral sunscreen actives
provides even coverage and superior protection without
drying the skin. Floramac 10 evenly disperses the zinc
oxide and titanium dioxide to improve the sunscreen
efficacy, boosting static SPF and improving skin feel.
A. Cyclomethicone (and) Propylene Carbonate (and)
Disteardimonium Hectorite (Bentone Gel VS-5PC V
(HV), Elementis) 2.50% w/w
Cyclopentasiloxane qs
B. Titanium Dioxide (and) Dimethicone (and) Hexyl Laurate (and)
PEG-10 Dimethicone (and) Polyglyceryl-4 Isostearate (and)
Stearic Acid (and) Alumina (UV Cut TiO2-41-DM,
Grant Industries Inc.) 15.00
Zinc Oxide (and) Dimethicone (and) PEG-10 Dimethicone
(UV Cut ZnO-61-DM, Grant Industries Inc.) 25.00
Ethyl Macadamiate (Floramac 10, Floratech) 12.00
Cetyl PEG/PPG-10/1 Dimethicone (Gransurf 90,
Grant Industries Inc.) 2.50
Polymethylsilsesquioxane (Gransil PSQ, Grant Industries Inc.) 2.50
Tocopheryl Acetate 0.20
Phenoxyethanol qs
C. Water (aqua) 10.00
Glycerin 2.00
1,3-Butylene Glycol 2.00
Procedure: Slowly combine A with stirring. Once mixture is a smooth, uniform gel,
shift to moderate propeller mixing. Add B to A in the order listed with moderate
propeller agitation. Once combined, mix with moderate homomixing agitation until
uniform. In a separate container, mix C until uniform. Very slowly add C to AB with
moderate homomixing agitation until smooth.
UV DEFENSE MILK SPF 38
(Grant Industries Inc.)
A. Water (aqua) 20.00% w/w
Acrylates/C10-30 Alkyl Acrylate Crosspolymer
(Carbopol ETD 2020 Polymer, Lubrizol Advanced
Materials, Inc.) 0.15
Xanthan Gum (Vanzan NF, Vanderbilt Minerals LLC) 0.05
Triethanolamine 0.15
Water (aqua) 17.15
Butylene Glycol 2.00
Glycerin 10.00
Sodium Benzoate 1.25
B. Cyclopentasiloxane 10.00
Caprylic/Capric Triglyceride (Protachem CTG, Protameen
Chemicals Inc.) 5.00
Dimethicone 3.00
Cyclopentasiloxane (and) Dimethicone (Gransil 314,
Grant Industries Inc.) 2.00
Stearoxymethicone/Dimethicone Copolymer (Gransil VX-401,
Grant Industries Inc.) 1.00
C. Simmondsia Chinensis (Jojoba) Seed Oil 1.00
Lauryl Glucoside (Plantacare 1200 UP, BASF SE) 1.50
Tocopherol Acetate 0.25
Phenoxyethanol 0.50
D. Titanium Dioxide (and) C12-15 Alkyl Benzoate (and)
Cyclopentasiloxane (and) Stearic Acid (and)
Polyhydroxystearic Acid (and) Alumina
(UV Cut TiO2-55-AC, Grant Industries Inc.) 25.00
100.00
Procedure: Combine A in the main kettle and mix at 70°C until all solids are dissolved.
Add B in order into the main kettle. Combine C in a support kettle and heat to
70°C until all solids are dissolved. Transfer support kettle into main kettle while
mixing. Add D into the main kettle and homogenize at 1,500-2,000 rpm until
uniform; note: sodium benzoate in A is a 20% aq. soln.
| DM30
3/18/20 2:40 PM
 EXPANDED Sun Care Formulary
ZINC FLUID, SPF-40
(Grant Industries Inc.)
A. Water (aqua) 12.00% w/w
Propanediol 7.00
Benzyl Alcohol (and) Salicylic Acid (and) Glycerin (and) Sorbic
Acid (Geogard ECT, Lonza Home & Personal Care) 1.00
Water (aqua) (and) Boswellia Serrata Extract (and) Centella
Asiatica Extract (and) Betula Alba Extract (and) Polygonum
Cuspidatum Root Extract (and) Phenoxyethanol (and)
Sodium Benzoate (Youth 360 BCR, Bio Component
Research) 3.00
Simethicone 0.10
Tromethamine 0.30
Polysorbate 20 0.10
B. C12-15 Alkyl Benzoate (Finsolv TN, Innospec) 4.50
Coco-Caprylate/Caprate (Cetiol LC, BASF SE) 3.00
Ethylhexyl Palmitate 3.00
Polyglyceryl-6 Polyricinoleate (and) Polyglyceryl-10
Dioleate (Gransurf PG-14, Grant Industries Inc.) 8.00
Zinc Oxide (and) Caprylic/Capric Triglyceride (and)
Polyhydroxystearic Acid (UV Cut ZnO-68-CG,
Grant Industries Inc.) 25.00
Lecithin 1.00
Isododecane (and) Disteardimonium Hectorite (and)
Propylene Carbonate (Bentone Gel ISD V, Elementis) 7.00
C. Dimethicone (and) Polysilicone-11 (and) Butyrospermum
Parkii (Shea) Butter (and) Water (aqua) (and) Glycerin
(and) Decyl Glucoside (Gransil SiW-038,
Grant Industries Inc.) 10.00
Isododecane (and) Polymethylsilsesquioxane/
Trimethylsiloxysilicate (Granresin MQI-T50,
Grant Industries Inc.) 10.00
Polymethylsilsesquioxane (Gransil PSQ, Grant Industries Inc.) 3.00
Aluminum Starch Octenylsuccinate 2.00
100.00
Procedure: Weigh B in main kettle equipped with homogenizer. Heat to 80-85°C
and mix until uniform. Weigh A in side kettle. Heat to 70-75°C and mix well. Once
each is at temperature, add A to main kettle and mix until uniform. Add C and mix
until uniform. Switch to side sweep agitation and cool to RT.
BE GONE BLUES ALOE ZNO
SPF 30 SUNSCREEN
(The Hallstar Company)
This formulation was designed to provide SPF 30
performance. It is water-resistant, preservative-free and
can be customized with natural butters and oils. The
oil-extracted active Blue Oléactif incorporates anti-blue
light, anti-pollution, protective and curative effects.
In vitro analysis delivered SPF ~33, PFA (PPD) ~12
performance with a critical wavelength of 376 nm.
A. Cocos Nucifera (Coconut) Oil (and) Aloe Barbadensis Leaf
Extract (Biochemica Aloe Butter, The Hallstar Company) 40.00% w/w
Glycine Soja (Soybean) Oil (and) Polyglyceryl-3 Diisostearate
(and) Oryza Sativa (Rice) Extract (Blue Oléoactif,
The Hallstar Company) 1.00
Polyhydroxystearic Acid 0.60
Prunus Amygdalus Dulcis (Sweet Almond) Oil
(Biochemica Sweet Almond Oil, The Hallstar Company) 20.40
Butyloctyl Salicylate/Titanium Dioxide/C12-15 Alkyl
Benzoate/Ethylhexyl Methoxycrylene/Triceteareth-4
Phosphate/Dimethicone Crosspolymer/Silica
(HallBrite EZ-FLO TDX Plus, The Hallstar Company) 25.00
B. Sorbitan Olivate (Olivem 900, The Hallstar Company) 3.00
C. Silica, Spherical 10.00
100.00
DM31 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020
CT2004_Sun_Care_Frmlry_fcx.indd 74
Procedure: Combine A and heat to 75°C with mixing. Add B with mixing. When AB
is uniform, add C to batch. When C is uniform, start cooling. Stop mixing when
batch is below 60°C; properties (25°C): appearance = smooth, white cream.
OLIVE AND LIME ANTI-SAND
MINERAL SUNSCREEN SPF 50
(The Hallstar Company)
This formulation was designed to provide globally
acceptable, anti-sand SPF 50 performance. Non-sticky
and fast-absorbing, the water-resistant formula has a
dry finish, which allows sand to brush off the skin with
ease. It is preservative-free and can be customized with
natural butters and oils. Biochemica Olive Butter and
Biochemica Lime Butter help to soften, moisturize and
rejuvenate skin, and evoke a sunshine-like scent. In vitro
analysis delivered SPF ~55, PFA (PPD) ~17 performance
with a critical wavelength of 378 nm. Water resistance
surpassed 4 hr during in-house in vitro testing.
A. Olea Europaea (Olive) Fruit Oil (and) Hydrogenated
Vegetable Oil (Biochemica Olive Butter,
The Hallstar Company) 34.00% w/w
Prunus Amygdalus Dulcis (Sweet Almond) Oil (and)
Hydrogenated Vegetable Oil (and) Citrus Aurantifolia
(Lime) Peel Oil (Biochemica Lime Butter, The Hallstar
Company) 3.00
Polyhydroxystearic Acid 0.60
Olea Europaea (Olive) Fruit Oil (BioChemica Olive
Oil-Ultra Refined, The Hallstar Company) qs to 100.00
Butyloctyl Salicylate/Titanium Dioxide/Triceteareth-4
Phosphate/Dimethicone Crosspolymer/Silica
(HallBrite EZ-FLO TDX, The Hallstar Company) 14.00
B. Zinc Oxide 13.00
C. Sorbitan Olivate (Olivem 900, The Hallstar Company) 5.00
Silica 14.00
Procedure: Combine A in main vessel. Heat to 75°C with mixing. Add B with mixing.
When uniform, add C with mixing. When uniform, begin cooling. Stop mixing at
60°C; properties: appearance = soft, off-white cream.
VERY WATER RESISTANT
SUNSCREEN SPF 20
(Innospec)
This very water resistant SPF 20 sunscreen lotion
features ethylene/VA copolymer as the waterproofing
agent.
A. Water (aqua) qs to 100.00% w/w
B. Disodium EDTA 0.10
C. Carbomer 0.25
Acrylates/C10-30 Alkyl Acrylate Crosspolymer 0.20
Propylene Glycol 2.00
D. Isononyl Isononanoate 2.50
Ethylhexyl Methoxycinnamate 7.00
Benzophenone-3 6.00
Cetyl Alcohol 0.75
Stearic Acid 1.25
E. Ethylene/VA Copolymer (Sensymer E, Innospec) 2.25
F. Triethanolamine 0.40
Water (aqua) 2.00
G. Preservatives qs
Procedure: Charge A into main beaker. Dissolve B into A. Start heating AB to 75-
80˚C. Disperse C into AB individually, allowing enough time between dispersion
so the polymer hydrates properly. Separately, blend D and heat to 75-80˚C with
3/18/20 2:40 PM

propeller mixing to obtain a clear phase. Add E to D and continue heating to
slightly over 95˚C. At 75-80˚C, form emulsion by adding ABC to DE with vigor-
ous propeller mixing. Add F to batch. Homogenize batch for 1-2 min at 3,500
rpms and return to propeller mixing. Cool and add G below 50˚C. Allow formula
to equilibrate for 24 hr.
PROTECTIVE SUN OIL
(Lucas Meyer Cosmetics)
This sun protection oil features MeliNOIL, a sunless
tanning agent. It imparts an SPF 10 in vitro, is non-
greasy, and it protects and nourishes the skin.
A. Prunus Amygdalus Dulcis (Sweet Almond) Oil 7.50% w/w
Ethylhexyl Salicylate 5.00
Simmondsia Chinensis (Jojoba) Seed Oil 15.00
Caprylic/Capric Triglyceride 7.50
Phospholipids (and) Glycine Soja (Soybean) Oil (and) Glycolipids
(and) Glycine Soja (Soybean) Sterols (Amisol Trio, Lucas
Meyer Cosmetics) 2.00
Triheptanoin 8.90
Cetyl Ethylhexanoate 35.10
Butyl Methoxydibenzoylmethane 3.00
Octocrylene 5.00
Ethylhexyl Methoxycinnamate 5.00
B. Fragrance (parfum) 0.80
Tocopherol (and) Helianthus Annuus (Sunflower) Seed Oil
(Vitapherole E1000, VitaeNaturals) 0.20
Isopropyl Palmitate (and) Lecithin (and) Water (aqua) (and)
Acetyl Hexapeptide-1 (MeliNOIL, Lucas Meyer Cosmetics) 5.00
100.00
Procedure: Prepare A and heat at 70-80°C under slow stirring. When mixture is
homogeneous, cool under medium stirring. Add B (one by one) below 40°C.
AGE DEFENSE CREAM
(Mibelle Biochemistry)
A. Water (aqua) 61.00% w/w
Disodium EDTA 0.10
Aminomethylpropanediol 3.00
Ethoxydiglycol 2.00
B. Ceteth-20 (and) Cetyl Alcohol (and) Glyceryl Stearate
(and) Steareth-20 (Emulium Delta, Gattefossé SAS) 4.00
Benzyl Alcohol 0.50
Benzoic Acid 0.20
Tocopheryl Acetate 0.20
Hydroxyethyl Acrylate/Sodium Acryloyldimethyl Taurate
Copolymer 0.30
Olea Europaea (Olive) Fruit Oil 1.00
Hydrogenated Vegetable Oil 1.00
Stearyl Alcohol 0.80
Myristyl Lactate 2.00
C10-18 Triglycerides 2.00
Hydrogenated Ethylhexyl Olivate 4.00
Hydrogenated Olive Oil Unsaponifiables 4.00
Dimethicone 0.80
C. Water (aqua) 10.00
Maltodextrin (and) Lecithin (and) Water (aqua) (and)
Coenochloris Signiensis Extract (Snow Algae Powder,
Mibelle Biochemistry) 3.00
D. Fragrance (parfum) 0.10
100.00
Procedure: Mix A until dissolved and heat to 70°C. Mix B and heat to 70°C. At
70°C, combine A and B under strong agitation and homogenize. Cool under
agitation. Combine C. Add C to batch below 40°C. Add D to batch. If necessary
adjust pH to 5.5-6.5 using E.
Vol. 135, No. 4 | April 2020 Cosmetics & Toiletries®
CT2004_Sun_Care_Frmlry_fcx.indd 75
EXPANDED Sun Care Formulary
AGELESS COMPLEX
(Sabinsa Corp.)
This formula features Sabinsa’s AgeLess Complex DCx
ingredient, with skin-whitening and collagen-building
properties.
A. Water (aqua) 90.25% w/w
Disodium EDTA 0.05
Glycerin 2.00
Carbomer 0.50
B. Aminomethyl Propanol 0.20
Water (aqua) 2.00
C. Water (aqua)/Niacinamide/Acetyl Glucosamine/Tocopheryl
Acetate/Hordeum Vulgare Extract/Glycerin/Polysorbate
20/Butylene Glycol/Lecithin/Pterocarpus Marsupium
Bark Extract/Phenoxyethanol/Methylisothiazolinone/
Caprylyl Glycol/Decylene Glycol/Tetrasodium EDTA/
Acrylates/C10-30 Alkyl Acrylate Crosspolymer/
Tetrahydropiperine (AgeLess Complex DCx, Sabinsa Corp.) 3.00
D. Dimethicone 1.00
Phenoxyethanol 1.00
E. Fragrance (parfum) qs
100.00
Procedure: Weigh all ingredients. Add ingredients of A in order. Add B to A and mix
well to create a thick gel. Add C to AB and mix well. Add D and E to ABC and
mix well. Adjust the pH of the product to between 5.5-6.5. Store in a cool and
dry place, protected from direct sunlight, and shake well before use.
SUN LOTION SPF 30 (O/W)
(schulke)
A. Glycerin (and) Lauryl Glucoside (and) Polyglyceryl-2
Dipolyhydroxystearate (Eumulgin VL75, BASF SE) 2.00% w/w
Hydrogenated Dimer Dilinoleyl/Dimethylcarbonate Copolymer 1.00
Octocrylene (Eusolex OCR, EMD Chemicals Inc.-RONA
Cosmetic Business Unit) 10.00
Butyl Methoxydibenzoylmethane (Eusolex 9020, EMD
Chemicals Inc.-RONA Cosmetic Business Unit) 3.00
Tocopherol 0.50
Sodium Cetearyl Sulfate (Lanette E, BASF SE) 0.75
Glyceryl Stearate 1.00
Pentaerythiryl Distearate (proposed) (Cutina PES, BASF SE) 2.00
Cetearyl Alcohol (Lanette O, BASF SE) 3.00
C12-15 Alkyl Benzoate 5.00
Dibutyl Adipate (Cetiol B, BASF SE) 3.00
Dicaprylyl Carbonate (Cetiol CC, BASF SE) 1.00
Butyrospermum Parkii (Shea) Butter (Cetiol SB 45, BASF SE) 2.50
B. Water (aqua) 48.25
Titanium Dioxide (and) Silica (Eusolex T-AVO, Merck KGaA) 6.00
Glycerin 5.00
C. Phenoxyethanol (and) Ethylhexylglycerin (euxyl PE 9010,
schulke) 1.00
D. Alcohol Denat. 5.00
100.00
Procedure: Heat A to 80-85°C and stir until uniform. Heat B separately to 80-85°C
and add to A while stirring. Allow emulsion to cool while stirring continuously.
Avoid incorporation of air. Homogenize with a suitable dispersion (e.g. Ultra
Turrax) until approx. 55°C. Stir while cooling to 40°C. Add C then D one after
another. Stop stirring at 30°C; properties: pH value = approx. 6.9; viscosity
(Brookfield RVF, 23°C, spindle 5, 10 rpm) = 15,000 mPa.s.
| DM32
3/18/20 2:40 PM
 EXPANDED Sun Care Formulary

W/O SUNSCREEN EMULSION SPF 30 Procedure: (Note: The formula and procedure shown here will create the SPF 15
variation of this formula; see below for variations to create the SPF 30 formula.)
(schulke) Heat A to 75-80°C and add B, mixing until dissolved. Add C to AB and disperse
A. Cetyl PEG/PPG-10/1 Dimethicone (Abil EM 90, well using high mechanical agitation, e.g., dissolver or homogenizer. Add D to ABC
and stir well. Mix E and heat to 80-85°C. Add E to ABCD while stirring well and
Evonik Industries AG) 5.00% w/w
form a homogenous emulsion. Cool slowly to 40-45°C while stirring rapidly. Add
Hexyldecanol (Eutanol G-16, BASF SE) 3.00
fragrance if desired and cool to RT while mixing slowly. For SPF 30, change the fol-
Dimethicone/Dimethicone Crosspolymer (Dow Corning lowing amounts: polyhydroxystearic acid to 0.38% w/w; ZnO product to 20.00%
EL-9140 DM Silicone Elastomer Blend, Dow Corning Corp.) 2.50 w/w; xanthan gum to 0.40% w/w; and water in the final phase to 55.82% w/w.
C12-15 Alkyl Benzoate (Finsolv TN, Innospec) 5.00
Cetyl Dimethicone 2.00
Ethylene/VA Copolymer
C12-15 Alkyl Benzoate (and) Stearalkonium Hectorite (and)
3.00 SPF 30 SHEER TOUCH FORMULATION
Propylene Carbonate (Bentone Gel TN V, Elementis) 5.00 (Ultra Chemical Inc.)
Butyloctyl Salicylate (HallBrite BHB, The Hallstar Company) 7.50
B. Zinc Oxide (and) Caprylic/Capric Triglyceride (and) Using a mineral-based sunscreen never felt so good. This
Polyhydroxystearic Acid (and) Triethoxycaprylylsilane Sheer Touch sunscreen applies to the skin with excellent
(GCP65HP1, Kobo Products Inc.) 20.00 spreadability for full coverage, and offers a transparent
C. Titanium Dioxide (and) Water (aqua) (and) Polyglyceryl-2 and luxurious soft finish after-feel. Consumers will be
Caprate (and) Sucrose Stearate (and) Simmondsia protected from UV thanks to Zano 20 Plus, all while
Chinensis (Jojoba) Seed Oil (and) Stearic Acid (and) having a good sensorial experience. It is recommended
Alumina (and) Glyceryl Caprylate (and) Squalane that all formulations are challenge-tested following the
(Solaveil XT-40W, Croda) 6.00 standards of your company.
Water (aqua) qs to 100.00
Butylene Glycol 3.00 A. Caprylyl Methicone/PEG-12 Dimethicone/PPG-20
Sodium Chloride 0.50 Crosspolymer (Dow Corning EL-7040 Hydro Elastomer
Hydroxyethylcellulose 0.75 Blend, Dow Corning Corp.) 23.00% w/w
D. Preservatives qs Tocopheryl Acetate 1.00
B. Dimethicone 20.00
Procedure: Combine A. Heat to 80°C and mix until solids are melted and dispersed.
Ethylhexyl Methoxycrylene (SolaStay S1, The Hallstar
Add B to A and mix until uniform. Keep temperature at 75-80°C. Homogenize
Company) 1.70
for 3 min at 3,500 rpm. Return to mixing. Combine C one by one. Heat to 75°C
and mix until uniform. Slowly add C to AB and mix to uniformity. Cool to 40°C.
Butyloctyl Salicylate (HallBrite BHB, The Hallstar Company) 4.00
Homogenize for 5 min at 5500 rpm. Return to mixer and cool to RT. Zinc Oxide (and) Triethoxycaprylylsilane (Zano 20 Plus,
Ultra Chemical Inc.) 20.00
Menthyl Lactate (Frescolat ML, Symrise, Inc.) 0.20
SPF 15 (AND 30) MINERAL Benzyl Alcohol (and) Dehydroacetic Acid (and) Water (aqua)
(Isocide BAS, Lehvoss) 1.00
SUN CARE SPRAY C. Glycerin 3.00
Alcohol 5.00
(Ultra Chemical Inc.)
Fragrance (parfum) 0.30
Water (aqua) 20.80
Say hello to your next mineral sunscreen spray. While
100.00
zinc oxide sprays can sometimes be a challenge due
to particle size, this spray formula with Zano 10 Plus Procedure: Mix A while slowly stirring. Mix C in a separate beaker while slowly stir-
disperses evenly onto the skin with good transparency ring. Prepare B in a separate beaker while slowly stirring by mixing all but the
and without clogging the delivery nozzle during ZnO-based product while slowly stirring and heating to 40°C (do not exceed
50°C). When the mixture is homogeneous, gradually add the ZnO product under
application. Choose between two SPF options (see continuous mixing. Homogenize with a high-speed disperser. Add B to A while
procedure for details) for what best suits your brand. slowly stirring and homogenize at a slow speed. Add C to AB while slowly mixing
It is recommended that all formulations be challenge- and homogenizing. When a gel is obtained, homogenize at high speed (1-2 min)
tested following the standards of your company. with a high-speed disperser.
A. Coco-Caprylate (Cetiol C 5, BASF SE) 16.00% w/w
B. Polyhydroxystearic Acid (Dispersun DSP-OL100, Innospec) 0.28
C. Zinc Oxide (and) Triethoxycaprylylsilane (Zano 10 Plus,
Ultra Chemical Inc.) 10.00
D. PEG-8 Stearate (and) Glyceryl Stearate (and) Cetearyl
Alcohol (and) Sorbitan Oleate (Olivem LV Flex,
The Hallstar Company) 4.00
Tocopheryl Acetate 1.00
Benzyl Alcohol (and) Dehydroacetic Acid (and) Water
(aqua) (BiosControl Synergy BAS, Biophil Group) 1.00
E. Phytic Acid 0.20
Lauroyl Lysine (Amihope LL, Ajinomoto North America, Inc.) 0.20
Panthenol 1.00
Xanthan Gum 0.30
Water (aqua) 66.02
100.00

DM33 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

CT2004_Sun_Care_Frmlry_fcx.indd 76 3/18/20 2:40 PM

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 Advertiser Index | C&T ®

The Definitive Peer-Reviewed Cosmetic Science Resource

The Definitive Peer-Reviewed
Cosmetic Science Resource

April 2020 |
Volume 135, number 4

Acme Hardesty Co., Inc. Croda, Inc. Lucas Meyer Cosmetics

57 9 7
sales@acme-hardesty.com marketing-usa@croda.com info@lucasmeyercosmetics.com
www.acme-hardesty.com www.crodausa.com www.lucasmeyercosmetics.com

Ashland Specialty Ingredients Evonik Mibelle AG Biochemistry

71 33 17
www.ashland.com personal-care@evonik.com info@mibellebiochemistry.com
www.elements-of-care.com www.mibellebiochemistry.com

BASF
63
yvonne.specht@basf.com Gattefossé USA Sabinsa Corp.
37 3
www.carecreations.basf.com ebrun@gattefossecorp.com info@sabinsa.com
www.gattefosse.com www.sabinsacosmetics.com

Bio-Botanica, Inc.
C2
info@bio-botanica.com Grant Industries schülke, Inc.
1 15
www.bio-botanica.com info@grantinc.com info@schuelke.com
www.grantinc.com www.schuelke.com

Biocogent LLC
31
info@biocogent.com Greentech SA Silab
45 29
www.biocogent.com greentech@greentech.fr silab@silab.fr
www.greentech.fr www.silab.fr

Campo Research Pte Ltd.

10
sales@campo-research.com Ichimaru Pharcos Co. Ltd. Siltech
69 53
www.campo-research.com gifu@ichimaru.co.jp www.siltechpersonalcare.com
(p. 11) www.ichimaru.co.jp

Voyant Beauty
C3
Centerchem, Inc. Ikeda Corp. info@voyantbeauty.com
C4 36
cosmetics@centerchem.com info@ikeda-america.com www.voyantbeauty.com
www.centerchem.com www.ikeda-corp.co.jp

Wacker Chemie AG
67
Contipro Innospec Ltd. www.wacker.com
19 5
www.contipro.com americas-pc@innospecinc.com
www.innospecinc.com

72 | www.CosmeticsandToiletries.com Vol. 135, No. 4 | April 2020

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