EXPERIMENTAL

NOTES

OptimaTM 8000 ICP-OES

ICP-OES-Pharma

Author
Sachin Salunkhe

Application Specialist Inorganic

Customer Knowledge Centre for Analytical Sciences
PerkinElmer (India) Pvt. Ltd.
Thane 400 615 India.
Email: application.india@perkinelmer.com

Analysis of Nutrient Elements in

Multi Vitamin Supplements using
Inductively Coupled Plasma Optical
Emission Spectrometer (ICP-OES)
Abstract
Multivitamin supplements are used to overcome nutritional deficiencies. We require
all the nutrients in their appropriate limits for optimum health. Since our diets cannot
provide all of the nutrients, multivitamin supplements aid/ boost our immune system.
The supplements should be tested and analyzed for its contents for potency. This
experimental note demonstrates the variety of unique features of Perkin Elmer
OptimaTM 8000 ICP-OES that enabled the accurate analysis of nutrient elements in high
matrix samples like multivitamin supplements.

Sample Preparation
Sample Preparation: Finely powdered the Multi Vitamin tablets,
and weighted approximately 3.5 g of sample and transferred to
250mL of glass volumetric flask. Slowly added 25 mL of aquaregia
(3:1= HCl:HNO3) solution in 5 mL increments followed by mixing.
Boiled the content on hot plate for almost 1 hour. Then removed
the flask from heat, cooled and diluted the solution to volume
with ASTM grade I water. The sample solution was prepared
separately for selenium. The sample was digested for NMT 15
minutes.
Standards Preparation: Calibration standards were prepared
as below.
Diluent used: 10% Aquaregia prepared in ASTM type I water.
Stock standard 1 (8 elements): Prepared a mixture of 5 mL of
1000 ppm standard of each Ca, Fe, K, Zn, Mg, Mn, Cu and P and
diluted to 50 mL with diluent. (Resulting concentration: 100 mg/L
of each)

Stock standard 2 (6 elements): Prepared a mixture of 0.5 mL of

1000 ppm standard of each Cr, Mo, Se, Ni, Sn and V and diluted
to 50 mL with diluent. (Resulting concentration: 10 mg/L of each)
Working Standards Concentration: Ca, Fe, K, Zn, Cu, Mg, Mn,
P: 1, 5, 10, 50, 100 mg/L; Cr, Mo, V, Ni, Se, B, Sn: 0.1, 0.5, 1, 3
mg/L.
Internal standard: Prepared a mixture standard of 1000mg/L of
Yttrium and 1000mg/L of scandium in 5% HNO3 solution and
diluent (1:1:198), and mixed.

Instrumental conditions
Optima

TM

8000 Optimized Experimental Conditions

Plasma gas flow

8 L/min

Auxiliary gas flow

0.4 L/min

Nebulizer gas flow

0.7 L/min

RF power

1500 Watts

Viewing height

15 mm

Plasma view

Axial/Radial

Read parameters

Auto (1 to 5(Min-Max))

Peristaltic pump flow rate

1.5 mL/min

Processing Peak

Area/Height

Calibration

Linear Calculated Intercept

Spray Chamber

Cyclonic Glass

Nebulizer

Concentric high solid

Injector

Alumina 2.0 mm i.d.

Quartz torch

1-slot

Analytical results
The digested samples were analyzed using Perkin Elmer
OptimaTM 8000 ICP-OES equipped with concentric high solid and
cyclonic spray chamber. Yttrium was used as the internal standard
to compensate for the viscosity and surface tension effects
between standards and sample. The three point calibration curve
gave correlation coefficient of 0.999 for all the elements analysed.
After verifying the calibration curve by using a quality control
check standard (procured from a second source) at the midpoint
of calibration, the digested samples were aspirated. A spike
recovery study was carried out in sample to ensure the validity of
the method developed. The spike recoveries obtained were in the
range of 90-110% for all the elements. The repeatability obtained
was good which confirmed the effectiveness of sample preparation
stage. The results of analysis are given in table below.

Element, Wavelength,
nm

Each coated tablet contains

Results for sample

Labeled value

Ca 315.887

161

160

162 mg

Fe 238.204

17

16

18 mg

K 766.490

83

83

80 mg

Zn 213.857

14

14

15 mg

Cu 327.393

2 mg

Mg 279.077

97

96

100 mg

Mn 259.372

2 mg

P 214.914

105

103

109 mg

Cr 267.716

110

113

120 mcg

Mo 202.031

71

73

75 mcg

V 310.230

10 mcg

Se 196.026

20

23

20 mcg

Sn 189.927

10 mcg

Ni 231.604

5 mcg

Conclusion
ICP-OES is an excellent technique for the determination
of the elements in high matrix samples like multivitamin
supplements as it provides good detection limit and wide
range of linearity. The dual view option of the OptimaTM
8000 ICPOES aided in analyzing both the high and low
concentration for different elements in a single run
without any further sample preparations like dilution or
preconcentration. An accurate and highly reproducible
method was developed for the analysis of minerals in
supplements products.