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Food Chemistry 221 (2017) 969–975

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Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem

Bioactives of coffee cherry pulp and its utilisation for production


of Cascara beverage
Andrea Heeger a,b, Agnieszka Kosińska-Cagnazzo a,⇑, Ennio Cantergiani c, Wilfried Andlauer a
a
Institute of Life Technologies, HES-SO Valais Wallis, University of Applied Sciences and Arts Western Switzerland, Route du Rawyl 47, CH-1950 Sion, Switzerland
b
Department of Nutrition and Food Sciences, University of Bonn, Endenicher Allee 11-13, D-53115 Bonn, Germany
c
Carasso-Bossert SA, Rue des Sablières 4-6, CH-1217 Meyrin, Switzerland

a r t i c l e i n f o a b s t r a c t

Article history: Coffee cherry pulp is a by-product obtained during coffee production. Coffee cherry pulp contains consid-
Received 12 April 2016 erable amounts of phenolic compounds and caffeine. An attempt to produce Cascara, a refreshing bever-
Received in revised form 15 November 2016 age, has been made. Six dried coffee pulp samples and a beverage called Cascara produced in Switzerland
Accepted 15 November 2016
out of one of those samples were investigated. Aqueous extraction of coffee pulps revealed a content of
Available online 16 November 2016
total polyphenols between 4.9 and 9.2 mg gallic acid equivalents (GAE)/g DM. The antioxidant capacity
was between 51 and 92 lmol Trolox equivalents (TE)/g DM as measured by the assay with ABTS radical.
Keywords:
Bourbon variety from Congo and maragogype variety showed highest caffeine contents with 6.5 and
Coffee cherry pulp
Bioactives
6.8 mg/g DM. In all samples chlorogenic acid, protocatechuic acid, gallic acid and rutin were present.
Polyphenols The beverage Cascara contained 226 mg/L of caffeine and 283 mg GAE/L of total polyphenols whereas
Caffeine antioxidant capacity amounted to 8.9 mmol TE/L.
HPLC Ó 2016 Elsevier Ltd. All rights reserved.
Functional beverage

1. Introduction skin, pulp, mucilage, parchment and parts of the silverskin are
removed during the de-hulling. The by-product that occurs is
Coffee is a beverage brewed from roasted coffee beans and called husk (Esquivel & Jiménez, 2012). The wet process separates
highly popular worldwide. Coffee plants are farmed in tropical ripened and unripe fruits in water; ripe fruit sink to the ground
areas whereas the beverage is consumed mainly in Europe and in whereas the unripe coffee cherries remain on the surface. After this
the United States. Arabica (Coffea arabica) and Robusta (Coffea separation pulp and the skin are removed with the aid of a pulper.
canephora) are the two varieties dominating the international Several authors call the obtained fraction pulp (Bressani, 1978;
markets. Murthy & Naidu, 2012; Pandey et al., 2000). The de-pulping is
Coffee cherry consists of skin, pulp, mucilage, parchment, silver- followed by a fermentation step where the mucilage and remnants
skin and coffee bean. Skin, also called pericarp, turns red in of the pulp are removed. The beans are then de-hulled; that means
ripeness. Below the skin there is the yellowish, fibrous and sweet the parchment is removed and dried (Esquivel & Jiménez, 2012;
pulp, the outer mesocarp. This covers a thin layer of mucilage, Pandey et al., 2000). More recently a third, semi-dry process has
the so called pectin layer. The next component is the parchment been developed, also known as honey process. In this semi-dry
or endocarp, which is followed by the silverskin. In the centre of process coffee cherries are de-pulped without subsequent
the fruit there is the coffee bean, the endosperm of the fruit fermentation step (Duarte, Pereira, & Farah, 2010). Coffee pulp is
(Esquivel & Jiménez, 2012). The coffee bean is used to produce the main residue obtained during wet and semi-dry processing
the actual coffee beverage. However, the processing of coffee (Bonilla-Hermosa, Duarte, & Schwan, 2014). Independently from
cherry into coffee beans is quite complex and generates a variety preparation process the obtained bean is roasted, generating typi-
of wastes. Ripened fruits are harvested and transformed by mainly cal coffee flavour, aroma and colour (Murthy & Naidu, 2012).
two ways of processing: wet or dry process. In the dry process the Fresh coffee cherries contain over 430 g of coffee cherry pulp
coffee cherries are sun-dried, followed by a de-hulling step. The per kg, the pulp represents nearly 30% of the dry matter (DM) of
the coffee berry (Bressani, 1978). With an average annual produc-
tion of ten million tons of coffee beans a huge amount of pulp as
⇑ Corresponding author.
by-product is generated. It is also worth mentioning that consider-
E-mail addresses: s7anheeg@uni-bonn.de (A. Heeger), agnieszka.kosinska@hevs.
ch (A. Kosińska-Cagnazzo), ecantergiani@carasso.ch (E. Cantergiani), wilfried. able amount of wastes comes from production of instant coffee as
andlauer@hevs.ch (W. Andlauer). well as from coffee brewing in restaurants (Jiménez-Zamora,

http://dx.doi.org/10.1016/j.foodchem.2016.11.067
0308-8146/Ó 2016 Elsevier Ltd. All rights reserved.
970 A. Heeger et al. / Food Chemistry 221 (2017) 969–975

Pastoriza, & Rufián-Henares, 2015). Due to the content of caffeine, The aim of this study was to quantify the bioactives and deter-
polyphenols and tannins the pulp causes environmental problems mine the antioxidant capacity of six dried coffee cherry pulp
in coffee producing countries if it is disposed without the necessary samples as well as to characterise Cascara ready-to-drink beverage
pre-treatment (Murthy & Naidu, 2012). Several attempts for a val- commercially produced in Switzerland from coffee cherry pulp.
orisation of the pulp have been made. For instance, coffee pulp can
be used for the production of compost and for vermi-composting
2. Materials and methods
(Murthy & Naidu, 2012; Pandey et al., 2000). The direct use for ani-
mal feed is limited due to the presence of anti-nutritional factors
2.1. Coffee cherry pulp and Cascara samples
such as caffeine and tannins (Esquivel & Jiménez, 2012). The addi-
tion of pulp to feed has been reported for ruminants, pigs chicken
Six coffee cherry pulp samples of different Coffea arabica vari-
and rabbits (Murthy & Naidu, 2012). A diet containing 30% coffee
eties, origin and processing and a commercial coffee cherry tea
pulp has been successfully tested for the fish tilapia (Bayne,
have been provided by La Semeuse SA (La Chaux-de-Fonds,
Dunseth, & Ramirios, 1976). There have been several attempts of
Switzerland). The samples of coffee cherry pulp varied strongly
reducing the content of antinutrients with physical, chemical and
in particle size (Fig. 1). The detailed information about the coffee
microbial methods, where the degradation with bacteria and fungi
variety, origin and type of process from which the samples are
seems to be most promising (Pandey et al., 2000). Also ensiling was
obtained is indicated in the Table 1. All coffee pulp samples were
reported to be an effective method (Ulloa Rojas, Verreth, Amato, &
grown in 2015 using organic cultivation. Cascara beverage was
Huisman, 2003). Coffee husk can also be used for the cultivation of
developed and produced at La Semeuse SA from the coffee cherry
mushrooms. By fermentation with Aspergillus, citric acid, gibberel-
pulp scarcely described, which was a mix of different varieties.
lic acid and enzymes have been produced (Murthy & Naidu, 2012;
The beverage was produced with 65.6 g DM coffee pulp per L of
Pandey et al., 2000). Yeasts and fungi produce bioethanol and
water, it was infused for 6.5 min at 90 °C. After infusion 71 g of
promising aroma compounds on coffee husk or pulp (Bonilla-
sugar and 5.7 mL of lemon juice was added per L of beverage.
Hermosa et al., 2014). There have also been attempts to use coffee
The beverage was bottled and pasteurised at 83 °C for 30 min.
pulp for biogas production (Pandey et al., 2000) and the production
of pellets for heating has been tested (Cubero-Abarca, Moya,
Valaret, & Tomazello Filho, 2014). Pyrolysis of coffee pulp impreg- 2.2. Reagents
nated with phosphoric acid yield a material with high adsorption
capacity. Hydrolysis of the pulp is another promising process to All reagents used were at least of analytical grade. Folin-
obtain sugars such as xylose, arabinose, fructose, glucose, sucrose Ciocalteu’s phenol reagent, gallic acid, (+)catechin, rutin, vanilic
and maltose (Murthy & Naidu, 2012; Pandey et al., 2000). Fresh acid, chlorogenic acid, syringic acid, p-coumaric acid, ferulic acid,
coffee pulp is a source of anthocyanins which could be used as quercetin, protocatechuic acid, gentisic acid, p-hydroxybenzoic
natural colorants for food (del Castillo, Fernandez-Gomez, acid, caffeic acid, sinapic acid, tyrosol, disodium hydrogen
Martinez-Saez, Iriondo, & Mesa, in press). Recently a coffee pulp phosphate, sodium chloride, potassium chloride, potassium dihy-
flour has been developed which has a fibre content of 18% drogen phosphate, 2,20 -Azobis(2-amidinopropane)dihydrochloride
(Ramirez Velez & Jaramillo Lopez, 2015). (AAPH), sodium fluorescein and caffeine were purchased from
Unroasted Arabica coffee beans (green coffee) contain 9–12.5% Sigma-Aldrich (Switzerland). Potassium persulfate, hydrochloric
of soluble carbohydrates, 45–63% of insoluble carbohydrates, acid, sodium carbonate and Trolox were bought from Acros Organ-
8.5–12% proteins, 15–18% lipids, 0.8–1.4% caffeine, 6.7–9.2% ics (Geel, Belgium). Absolute ethanol was obtained from Alcosuisse
chlorogenic acid, and 3–5.4% minerals (Belitz, Grosch, & (Bern, Switzerland). ()Epicatechin, caftaric acid and scopoletin
Schieberle, 2009). Coffee pulp contains about 50% of carbohydrates, were bought from Aktin Chemicals (China). 2,20 -azino-bis(3-
10% protein, 20% fibres, 2.5% fat, and 1.3% caffeine, it also contains ethylbenzothiazoline-6-sulphonic acid) (ABTS) was from Southern
phenolic compounds (Pandey et al., 2000). The composition of Biotech (USA). Formic acid was obtained from Merck (Germany),
phenolic compounds in coffee pulp has been a subject of some Acetonitrile from Macron (Macron Fine Chemicals, Poland). The
studies in recent years. Four major classes of phenolic compounds water was obtained with a Milli-Q system (Merck-Millipore,
identified were: flavan-3-ols (monomers and procyanidins), Germany).
hydroxycinnamic acids, flavonols, and anthocyanidins (Ramirez-
Coronel et al., 2004) with chlorogenic acid as predominant 2.3. Aqueous extraction of coffee cherry pulp
phenolic compound (Rodríguez-Durán et al., 2014). It was shown
that coffee cherry pulp is a potential source of antioxidants and Preliminary experiments (data not shown) indicated that the
phenolic compounds which should not be wasted. Since coffee particle size influenced the yield of bioactives extraction from cof-
cherry pulp and coffee beans contain similar components dried fee cherry pulp. Therefore all dried coffee cherry pulp samples
coffee cherry pulp can be used to produce a refreshing and stimu- were shred with a Moulinex ‘‘la moulinette xxl” (France). The par-
lating beverage called Cascara (cascara: Spanish word for husk). ticles were separated with a sieve w = 1.4 mm; d = 0.71 mm. Only
Cascara, also known as coffee cherry tea, is an infusion of dried cof- the particles < 1.4 mm were used for extraction.
fee cherry pulp. The approach to valorise food byproducts by The coffee cherry pulp samples (1.0 g) were extracted twice
preparing an infusion out of it, has already been described for other with 10 mL of hot water for 15 min at 85 °C in a water bath. Water
agricultural byproducts such as coffee silverskin (Martinez-Saez extracts were centrifuged at 3 220 g for 7 min with an Eppendorf
et al., 2014) or buckwheat hulls (Zielińska, Szawara-Nowak, & Centrifuge 5810 (Germany). The supernatants were collected in a
Zieliński, 2013). Functional beverages largely contribute to the 25 mL volumetric flask. A third extraction was performed with
globally growing market of functional food (Corbo, Bevilacqua, 4 mL of hot water in the ultrasonic bath for 15 min followed by
Petruzzi, Casanova, & Sinigaglia, 2014). The authors of the above centrifugation at 3 220 g for 10 min. The supernatant was filtered
cited review list the use of by-products of fruit and food industries into the flask and the volume was completed with water to
as functional ingredients as one of the main approaches in the area 25 mL. Extracts were made in triplicate. For HPLC analysis, the
of the research and innovation in the food field. Coffee silverskin extracts were filtered with Exapure 0.45 lm nylon filters
extract was utilised for production of antioxidant beverage for (Switzerland).The Cascara beverage was analysed as such after fil-
preventing fat accumulation (Martinez-Saez et al., 2014). tration with Exapure 0.45 lm nylon filter.
A. Heeger et al. / Food Chemistry 221 (2017) 969–975 971

Fig. 1. Appearance of six dried coffee cherry pulp samples. For the characteristics see Table 1.

Table 1
Horszwald and Andlauer (2011) with some modifications. The lat-
Coffee cherry pulp sample characteristics. ter method is based on an electron transfer reaction during which
phenolic and nonphenolic substances are reduced; however the
Sample Variety Origin Type of process
obtained result is traditionally called total polyphenols content
1 Bourbon Salvador Wet (Huang, Ou, & Prior, 2005). Each extract was analysed in triplicate.
2 Caturra Honduras Wet
3 Mixed varieties Honduras Semi-dry
Absorbance and fluorescence measurements were performed using
4 Catuai Honduras Semi-dry a Tecan Infinite M200 pro microplate reader (Switzerland).
5 Bourbon Congo Wet Microplates with 96 wells were purchased from Nunc (Nunc A/S,
6 Maragogype Honduras Semi-dry Ruskilde, Denmark). Transparent microplates were used to deter-
mine the absorbance and black microplates for fluorescence
measurements.
2.4. Dry matter content

The dry matter (DM) of coffee cherry pulp samples was deter- 2.5.1. ABTS assay
mined in duplicate with a halogen-balance (Mettler Toledo HG53 A stock solution of ABTS radical was produced by dissolving
Moisture Analyzer, Switzerland). The mass loss at 110 °C was 96 mg ABTS in about 20 mL of water, then adding 2.5 mL of potas-
determined gravimetrically. The results given in % of raw material sium persulfate solution (2.45 mmol/L) and finally filling to 25 mL
were used for the calculation of the results of individual analysis with water. The stock solution was left to rest overnight and stored
per g of DM. in the fridge. The stock solution was diluted in ethanol so that an
absorbance between 0.6 and 0.8 was obtained. The extracts and
Cascara beverage were diluted in ethanol. The wells of the micro-
2.5. Antioxidant capacity assays plate were filled with 20 lL of the diluted sample. Then 290 lL
of ABTS solution were added with the injector. The absorbance at
The antioxidant capacity was determined by the TEAC (Trolox 755 nm was measured after 6 min of incubation at 30 °C. Trolox
Equivalent Antioxidant Capacity) using ABTS method, the ORAC solutions in ethanol in the concentration range of 5–200 mg/L were
(Oxygen Radical Absorbance Capacity) method and total used as standards. The results are indicated as lmol Trolox equiv-
polyphenols method with Folin-Ciocalteu reagent as described by alents per g dry matter (TE/g DM).
972 A. Heeger et al. / Food Chemistry 221 (2017) 969–975

2.5.2. ORAC assay 3. Results and discussion


For the ORAC assay the extracts were diluted 1:50 or 1:100
with phosphate buffer (pH 7.4, 0.02 mmol/L) containing KCl The dry matter (DM) content of all coffee cherry pulp samples
(0.001 mmol/L) and NaCl (0.07 mmol/L). The microplate wells was determined in order to report the results on DM basis. The
were filled with 50 lL of diluted extracts and Cascara sample and results obtained were quite similar for all samples ranging
50 lL of 300 nmol/L fluorescein solution and 100 lL of 50 mmol/L between 90% and 93% of DM.
AAPH solution were added using the injectors of the microplate
reader. The microplate reader was kept at 37 °C. During 2 h the flu- 3.1. Antioxidant activity of coffee cherry pulp samples
orescence was measured every 2 min at excitation wavelength of
485 nm and emission wavelength of 520 nm. As standards Trolox The extraction of coffee cherry pulp was conducted in hot water
solutions in the concentration of 1–100 mg/L in phosphate buffer in order to simulate the condition of Cascara beverage production.
were used. Again results are indicated as lmol TE/g DM. The results of antioxidant capacity obtained in different methods
are reported in Fig. 2. The highest total polyphenols content
amounting to 9.17 mg GAE/g DM was observed for bourbon variety
2.5.3. Total polyphenols content originating from Congo. Other samples showed values between
The extracts were analysed according to the method with 4.85 mg GAE/g DM and 6.08 mg GAE/g DM. All measured values
Folin-Ciocalteu reagent. 25 lL of the extract or Cascara sample were lower than literature values for coffee cherry pulp ranging
was pipetted into wells of the microplate. To each well 250 lL of between 11 and 20 mg/g for a 70% methanol/water extract (Ulloa
diluted Folin-Ciocalteu reagent (2 + 30 with water) was automati- Rojas et al., 2003) and 122 g/kg for acidified aqueous methanol
cally added with the injector. After 10 min of incubation at room (Arellano-González, Ramírez-Coronel, Torres-Mancera, & Pérez-
temperature, 25 lL of sodium carbonate solution (5% in water) Morales, 2011). The explanation for these different extraction
was added to the wells. The plate was incubated for 20 min and yields is obvious: water/methanol and water/ethanol mixtures
absorbance was measured at 755 nm. As standards, solutions of have been shown to give higher extraction yields than water for
gallic acid in water in the range of concentration from 50 mg/L to different agricultural residues (Vijayalaxmi, Jayalakshmi, &
500 mg/L were prepared. The results are indicated as gallic acid Sreeramulu, 2015). Zakaria (2013) compared one coffee cherry
equivalent per g DM (mg GAE/g DM) of the coffee pulp sample. pulp sample prepared as a methanol/water (60:40) extract with
The result of the Cascara is given as mg gallic acid equivalent per an aqueous infusion. A methanol/water extract contained
litre (mg GAE/L). 27.61 mg GAE/g and the water extract of the same sample showed
22.75 mg GAE/g (Zakaria, 2013). The extraction with a methanol/
water mixture seems to be more effective than with hot water.
2.6. HPLC-DAD analysis of caffeine and phenolic compounds content For the ABTS test again coffee cherry pulp of bourbon variety
originating from Congo showed the highest antioxidant capacity
Samples were analysed by HPLC for the profile of polyphenols with 92.2 lmol TE/g DM (Fig. 2). Coffee cherry pulp of bourbon
and the caffeine content. For this analysis an Agilent 1220 Infinity variety originating from Honduras and of varietal mix from
series liquid chromatograph (Agilent Technologies, Santa Clara, CA, Honduras showed similar values amounting to 67.4 and 64.9 lmol
USA) with a 100  2.1 mm KinetexÒ 2.6 lm EVO C18 100Å column TE/g DM, respectively. The other samples ranged between 51 and
was used (Phenomenex, Torrance, CA, USA). The elution was 54 lmol TE/g DM. As expected, there is a good correlation between
conducted with a gradient of water with 1% aqueous formic acid total polyphenol content and ABTS values (R2 = 0.95).
(eluent A) and acetonitrile with 1% formic acid (eluent B). The sep- Also in the case of the ORAC assay there are the highest values
aration started with 100% A for 2 min, 2–25 min B was increasing of the antioxidant capacity for the coffee cherry pulp of bourbon
to 10%, 25–26 min B was kept at 10%, 26–30 min B 10–60%, B variety originating from Congo and for sample of varietal mix from
was kept for 5 min at 60%. From 35 min A was set back to 100%. Honduras with 274 lmol TE/g DM and 233 lmol TE/g DM, respec-
The detection was performed with a diode array detector at tively. The lowest antioxidant capacities were found for cattura,
260 nm, 280 nm, 320 nm and 340 nm. Undiluted extracts (three catuai and maragogype varieties originating from Honduras with
from each sample) and the Cascara (three samples) were filtered values between 136 and 153 lmol TE/g DM.
and 1 lL was injected onto the column. The individual polyphenols
and caffeine were identified by comparison of their retention times
and UV-spectra with those of the standards. The quantification was 300 30
a
made via external calibration. The following substances were used
as standards: caftaric acid, cafeic acid, chlorogenic acid, p-coumaric 250 a 25
antioxidant capacity [µmol TE/g DM]

total polyphenols [mg GAE/g DM]

acid, ferulic acid, sinapic acid, gallic acid, protocatechuic acid,


p-hydroxybenzoic acid, vanillic acid, gentisic acid, scopoletin, rutin, 200 b 20
quercetin, tyrosol, (+)-catechin, caffeine, syringic acid and c
(-)-epicatechin. Standards of p-hydroxybenzoic acid, tyrosol and 150
c c
15
sinapic acid were prepared in ethanol, all other standards in
water. 100 a a 10
b b b
b,c c c
c c c c
50 5
2.7. Statistical analysis
0 0
The results are presented as mean ± standard deviation for bourbon S. caturra H. mixed H. catuai H. bourbon C. maragogype H.
three individual extractions from each sample of coffee cherry pulp
Fig. 2. Antioxidant capacity of six samples of dried coffee cherry pulp evaluated by
and for three individual bottles for beverage. The significance of
ABTS , ORAC h and total polyphenols assays. Results are expressed as
difference was analysed using a one way ANOVA and a post hoc mean ± SD, n = 3. Different letters above the bars of the same colour denote
Tukey-Kramer test (Granato, de Araújo Calado, & Jarvis, 2014). significant difference between the samples at p < 0.05. S. – Salvador, H. – Honduras,
The differences were considered significant at p < 0.05. C.- Congo.
A. Heeger et al. / Food Chemistry 221 (2017) 969–975 973

Coffee cherry pulp of bourbon variety (Coffea arabica var. The caffeine contents of the six coffee cherry pulp samples var-
bourbon) processed with wet method was obtained from planta- ied between 3.4 and 6.8 mg/g DM. Bourbon variety from Congo and
tion in Salvador and Congo. The significantly higher results of maragogype variety showed highest caffeine contents with 6.5 and
antioxidant capacity were noticed for the sample from Congo. 6.8 mg/g DM whereas varietal mix from Honduras had the lowest
content. The caffeine values recorded in this work are within the
3.2. Content of polyphenols and caffeine in coffee cherry pulp samples same range or lower than caffeine contents found in literature that
vary between 5.4 and 18 mg/g. However, literature values were
Individual polyphenols and caffeine were determined by HPLC. obtained with different extraction methods (Clifford & Ramirez-
The most prominent compounds identified in the extracts Martinez, 1991; Ulloa Rojas et al., 2003).
are shown in Fig. 3. Chlorogenic acid and protocatechuic acid The sample used for the coffee cherry tea production (varietal
are the dominant polyphenols in all analysed samples. In total, mix from Honduras) showed second highest values for total
these compounds made up more than 80% of the determined polyphenols content and ORAC value. Yet it possessed the lowest
polyphenols. Gallic acid and rutin were present in all coffee cherry caffeine content of all investigated samples.
pulp samples as well, yet in much lower quantities (6 0.1 mg/g DM).
The exception was coffee cherry pulp of bourbon variety originat- 3.3. Bioactive content and antioxidant activity of Cascara
ing from Congo which contained 0.73 mg/g DM of gallic acid.
Again this sample showed the highest values for chlorogenic acid, Table 2 shows the content of caffeine and individual phenolic
gallic acid and protocatechuic acid content and for the sum of compounds in Cascara beverage and its antioxidant activity. The
determined polyphenols. The sum of individual polyphenols Cascara contained 226 mg of caffeine/L of beverage. Most
determined by HPLC correlated well with total polyphenol commonly consumed caffeine containing beverages are coffee
content determined by total polyphenols method (R2 = 0.97). The and tea. The difficulty in comparison of the obtained results with
presence of chlorogenic acid (42.2%), protocatechuic acid (1.6%) those reported for tea and coffee lies in the different brewing pro-
and rutin (2.1%) has already been reported by Ramirez-Martinez cedures which have strong effect on bioactive compounds content.
in fresh coffee pulp extracted with 80% methanol (Ramirez- Nevertheless, the ranges of bioactive contents reported for coffee
Martinez, 1988). The presence of catechin (2.2%), epicatechin (espresso, filter, instant, Turkish and Italian), silverskin tea, ready
(21.6%) and ferulic acid (1.0%) was reported there as well; to drink green tea beverage and buckwheat hull infusion were
however those substances could not be detected in this study. It compiled in the Table 2. Cascara contained more caffeine than sil-
is possible that epicatechin was degraded during processing and verskin drink, but most types of coffee are richer in this compound.
storage. Presumably, there were also differences in the extraction The caffeine content of Cascara was similar to the average value
efficiency. reported for black tea by Barone and Roberts (1996). Protocate-
Similarly as for the results of antioxidant capacity two samples chuic and chlorogenic acid were the dominant phenolic com-
of coffee cherry pulp of bourbon variety, both obtained with the pounds identified in Cascara, amounting to 85.0 and 69.6 mg/L,
wet process but from different plantation countries differ respectively. Also small amounts of gallic acid and rutin were
significantly in the content of individual phenolic compounds. This noted. Chlorogenic acids are dominant phenolic compounds of cof-
indicates that either there were differences within the execution of fee brews. Again their content depends strongly on the brewing
the wet process (e.g. de-pulping) or other factors like growing con- method and it might range from 150 to 3260 mg/L (Komes &
ditions (altitude, climate, soil and agricultural practices) or harvest Belščak-Cvitanović, 2014). Comparing with silverskin tea Cascara
time influenced the polyphenols content (Cheng, Furtado, Smyth, & was richer in chlorogenic acid.
Henry, 2016). For example, it was reported that coffee beans grown The Cascara beverage had also considerable antioxidant capac-
at higher altitude had higher content of chlorogenic acid and ity amounting to 3.02 and 8.86 mmol TE/L for ABTS and ORAC
caffeine, whereas rainfall had no significance for chlorogenic acid assay respectively. The antioxidant capacity of the beverage might
content (Cheng et al., 2016). be a result of activity of compound coming from coffee cherry pulp

8.0
a
7.0 a

6.0 b

5.0
content [mg/g DM]

c c

4.0 d
a
3.0
a

2.0 b
b
c a c
1.0 d d
0.73 a
c e b c b a c b c b
b
0.03 0.05 0.02 e 0.06 0.07 0.10 0.02 d 0.06 0.09 0.02 d 0.05
0.0
bourbon S. caturra H. mixed H. catuai H. bourbon C. maragogype H.

Fig. 3. Content of individual polyphenols (gallic acid &, protocatechuic acid , chlorogenic acid , rutin ) and caffeine h of six samples of dried coffee cherry pulp
determined by HPLC. Results are expressed as mean ± SD, n = 3, different letters above the bars of the same colour denote significant difference in the content of individual
compound between the samples at p < 0.05. Due to the very low bars representing gallic acid and rutin content the values were given.
974 A. Heeger et al. / Food Chemistry 221 (2017) 969–975

Table 2
Contents of caffeine, individual polyphenols and antioxidant activity of Cascara beverage in comparison to some literature data.

Cascara Coffeea Silverskin teab Green tea ready-to-drinkc Buckwheat hull infusiond
Caffeine content (mg/L) 226.4 ± 1.2 174–5400 50–190 n.r. n.r.
Phenolic compounds content (mg/L)
Gallic acid 4.3 ± 0.5 n.r. n.r. n.r. n.r.
Protocatechuic acid 85.0 ± 0.5 n.r. n.r. n.r. n.r.
Chlorogenic acid 69.6 ± 0.4 150–3260 20–30 n.r. 0.6
Rutin 6.1 ± 0.0 n.r. n.r. n.r. n.r.
Catechins n.r. n.r. 300–1000 n.r.
Antioxidant activity
ORAC (mmol TE/L) 8.86 ± 0.186 n.r. n.r. 6–22 n.r.
ABTS (mmol TE/L) 3.02 ± 0.006 6.97–54.1 n.r. n.r. n.r.
TPC (mg of GAE/L) 283 ± 12.0 250–18000 159–354e 450–1700 32f

Results of Cascara are expressed as means ± standard deviation of triplicate analysis; TE – Trolox equivalents, TPC – total phenolic content, GAE – gallic acid equivalents.
n.r. not reported in the cited study.
a
Ranges for brews prepared by different brewing techniques (Komes & Belščak-Cvitanović, 2014).
b
Ranges for beverages based on Arabica and Robusta silverskin extract 2.5 g/L (Martinez-Saez et al., 2014).
c
Ranges for four ready-to-drink green tea beverages from Brazilian market (Kodama, de Gonçalves, Lajolo, & Genovese, 2010).
d
Infusion prepared from 2 g of buckwheat hull with 200 ml of water (Zielińska, Szawara-Nowak, & Zieliński, 2013).
e
Expressed as chlorogenic acid equivalents.
f
Expressed as catechin equivalents.

and scarcely from lemon juice used for its production. The calcula- of the taste of the potential beverage made of this type of coffee
tions based on the literature data shows that 5.7 mL of lemon juice cherry pulp remains to be evaluated.
used for the production of 1 L of Cascara could contribute up to The utilisation of well-defined coffee cherry pulp, obtained
0.01 mmol TE/L to the final antioxidant capacity of the beverage under known conditions of processing but also cultivation might
(Pellegrini et al., 2003). The values obtained for Cascara in this help to develop a valuable and reproducible product. Definitely,
study were definitely lower than those reported for coffee brews those parameters could affect the bioactive compounds in the
but within the range for green tea ready to drink products by-products. However, it should not be forgotten that coffee cherry
(Kodama, de Gonçalves, Lajolo, & Genovese, 2010; Komes & pulp is a by-product. The parameters of coffee cultivation or
Belščak-Cvitanović, 2014). The coffee cherry tea contained processing will never be modified by the growers in order to
283 mg GAE/L of total polyphenols. This is about a third of the optimise the by-product quality. Finding possibility of coffee
amount of total polyphenols which Saura-Calixto and Goñi cherry pulp utilisation may help to avoid its dumping which causes
(2006) reported in a black tea (763 mg/L) and more than ten times environmental problems. At the same time the content of phenolic
less than the amount for coffee (3430 mg/L). A beverage made from compounds in pulp originating from different plantations will vary
coffee silverskin extract and buckwheat hull tea are other which should be taken into account for the reproducible produc-
beverages produced out of by-products. Buckwheat hull tea tion of the beverage.
contained a smaller amount of total polyphenols than Cascara with The samples of coffee cherry pulp obtained from coffee produc-
about 32 mg catechin equivalents/L (Zielińska et al., 2013). The ers from different parts of the world, differing in variety and type of
beverage prepared from coffee silverskin extract showed the total processing showed significantly different contents of phenolic
polyphenols content comparable to the Cascara with the values compounds and caffeine. Among the assessed samples, bourbon
of about 350 mg chlorogenic acid equivalent/L (eq. CGA/L) for variety originating from Congo had highest total polyphenol
Robusta coffee and about 150 mg eq. CGA/L for Arabica coffee content and antioxidant capacity and high caffeine content.
(Martinez-Saez et al., 2014).
The content of phenolic compounds obtained for Cascara was
Conflict of interest
compared with the sample of varietal mix from Honduras out of
which the Cascara was produced. The recovery rate of extraction
Ennio Cantergiani used to work for La Semeuse SA and devel-
performed carefully in the laboratory and that obtained during
oped the Cascara beverage. He did not participate in the study
the production process were similar for most of the compounds.
design or analytical part of the study. All other authors have no
Namely, contents of caffeine, gallic acid, protocatechuic acid and
conflict of interest.
rutin were shown to be similar for the coffee cherry tea and for
the water extract at 85 °C with yields between 95 and 102%. This
indicates that those substances are stable during pasteurisation Acknowledgments
and storage of the beverage. Surprisingly, the Cascara contained
much less chlorogenic acid than the calculated value (68%). Chloro- We thank La Semeuse SA for the providing of the dried coffee
genic acid was shown to partly form isomers and react with water cherry pulp samples and the Cascara. The technical assistance of
when heated under reflux as an aqueous solution (Dawidowicz & Isabelle Héritier is highly appreciated. The study was partly funded
Typek, 2010). Probably some of the losses of chlorogenic acid in by the University of Applied Sciences and Arts Western
the beverage were due to heating during the pasteurisation Switzerland thematic research program HealthFood.
process.
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