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Atomic Absorption
Authors:
Lee Davidowski, Ph.D.
Lorraine Foglio
PerkinElmer, Inc.
Shelton, CT 06484 USA

The Determination of
Minerals and Metals
in Multi-Mineral/MultiVitamin Tablets by Flame
Atomic Absorption
Spectroscopy

Introduction

There are many mineral dietary supplements
available in today’s marketplace to ensure
that mineral deficiencies do not occur in
one’s diet. The mineral content of these
products must be verified for quality
control (QC) purposes. Furthermore, the
Nutritional Labeling and Education Act of
1990 mandates accurate labeling of all
food supplements sold in the U.S. which
means accurate testing of the products
is mandatory. In many labs, this task is
accomplished by the technique of flame
atomic absorption spectroscopy (FAAS). FAAS has the advantages of lower initial
cost, low cost per analysis, and requires less operator training than many other
trace elemental techniques. The objective of this work is to demonstrate the
applicability of FAAS using the PerkinElmer® PinAAcle™ 900T to accomplish this
task. Seven elements are determined in two commercially available multi-mineral
tablets, a NIST® Standard Reference Material, and a commercial reference material
which simulates a mixed food diet.
Experimental
Instrumentation
The PinAAcle 900T flame and longitudinal Zeeman furnace
atomic absorption spectrometer controlled by WinLab32™
for AA software, running under Microsoft® Windows® 7,
was used for all analyses (PerkinElmer, Inc., Shelton, CT). A
high-sensitivity nebulizer (Part No. N3160112) with a spacer
was employed. Single-element Lumina™ hollow cathode
lamps (HCLs) were used and the instrumental operating
conditions for each element in this application are shown in
Table 1. A four-second integration time and three replicates
were used for all elements.

approximately one hour and warmed, not to boiling, on a
hot plate. Deionized water was then added to the volumetric
mark after removal of the magnetic stir bar. The sample
digestion solution was then filtered through Whatman®
46 paper (passes < 8 micron) to remove waxy undissolved
material, presumably from the tablet’s coating. The filtrate
was then analyzed, after appropriate dilution, against singleelement aqueous standards (PerkinElmer Pure) for elemental
quantitation. A Certified Reference Material Mixed Food
Diet (CRM-MFD) (High Purity Standards, Charleston, SC)
was prepared by dissolution, following the manufacturer’s
instructions, to an appropriate concentration for individual
elements.
All tablets also contained about 2 mg/tablet of silicon, much
of which may have remained undissolved. For an accurate
measurement of the silicon, HF (trace metal grade) and plastic
volumetric flasks should be employed for the dissolution.
For calcium and magnesium determinations, La(NO3)2
(reagent grade) was added to all standards, blank and
samples to a concentration level of 0.2% to remove chemical
inferences from other matrix elements. For potassium
determinations, CsCl (reagent grade) was added to all test
solutions to a concentration level of 0.2% as an ionization
buffer.

Figure 1. PinAAcle 900T atomic absorption spectrometer.

Results
Sample and Standard Preparation
One NIST® SRM 3280 Multi-vitamin/Multi-mineral Tablet and
two over the counter multi-vitamin/multi-mineral tablets were
coarsely ground. Nominally, 0.75 g were weighed out and
rinsed into a 1000 mL volumetric flask containing about
20 mL of ASTM® Type I deionized water (>16MΩ • cm).
Four mL of HCl (trace metal grade), two mL of HNO3 (trace
metal grade), and a magnetic stirring bar were then added
to the flask. This sample digestion solution was stirred for

All elements showed acceptable calibration criteria. The
results obtained for the FAAS analyses of the multi-vitamin/
multi-mineral tablets are shown in Table 2. The values are
corrected for laboratory sample dissolution steps and dilutions.
The commercial tablets were calculated and reported in mg/
tablet as this was the unit shown and guaranteed on each
label. All elements were found to be within the certified
range for the NIST® 3280 tablet. Both commercial tablets
showed good correlation to labeled quantity guaranteed by
the manufacturer.

Table 1. PinAAcle 900T Instrumental Parameters.
	

Element

Parameter	

Ca	

Mg	

K	

Fe	

Zn	

Cu	

Mn

Wavelength (nm)	

422.7	

285.2	

766.5	

248.3	

213.9	

324.8	

279.5

Slit Width (nm)	

0.7	

0.7	

0.7	

0.2	

0.7	

0.7	

0.2

Oxidant Flow (L/min)	

10	

10	

10	

10	

10	

8.7	

10

C2H2 Flow (L/min)	

2.5	

2.5	

2.2	

2.5	

2.0	

2.5

5	

1	

4	

4	

1	

4	

2

HCL Part Nos. 	

N3050114	

N3050144	

N3050139	

N3050126	

N3050191	

N3050121	

N3050145

Standard Part Nos.	

2

2.5	

Working Range (mg/L)	

N9303763	

N9300179	

N9303779	

N9303771	

N9300178	

N9300183	

N9303783
Table 2. Corrected FAAS results for one certified reference material and two commercial multi-vitamin/multi-mineral samples.
	
	
Element	

NIST® 3280	
(mg/g)	
Certified	

Found	

Commercial Tablet 1	
(mg/Tab)	
SD	

Label	

Found	

SD	

Commercial Tablet 2
(mg/Tab)
Label	

Found	

SD

Ca	

110.7	

107	

0.8	

162	

163	

0.6	

200	

211	

0.6

Mg	

67.8	

69.1	

0.2	

100	

107	

0.4	

100	

109	

0.4

K	

53.1	

53.8	

0.3	

80	

83.8	

0.4	

80	

90.7	

0.4

Fe	

12.35	

12.9	

0.05	

18	

19.1	

0.08	

n/a	

0.23	

0.006

Zn	

10.15	

10.1	

0.02	

15	

15.5	

0.04	

15	

15.2	

0.03

Cu	

1.4	

1.42	

0.01	

2	

2.19	

0.01	

2	

2.04	

0.01

Mn	

1.44	

1.48	

0.01	

2	

1.91	

0.01	

2	

2.04	

0.01

The results for the FAAS analysis of the Certified Reference
Material – Mixed Food Diet from High Purity Standards – are
given in Table 3. All elements were found to be within 5%
of the certified value, showing excellent agreement with the
reference material.
Table 3. Mixed Food Diet CRM results using aqueous
standards and FAAS on a PinAAcle 900T.
	
	

CRM-MFD
(mg/L)

Element	

Certified	

Found	

SD

Ca	

40	

39.8	

0.2

Mg	

12	

11.8	

160	

159	

0.005

Fe	

0.8	

0.802	

0.005

Zn	

0.3	

0.290	

0.001

Cu	

0.06	

0.061	

0.001

Mn	

0.2	

0.191	

The mineral content of multi-vitamin/multi-mineral tablets
must be determined in order to ensure the quality of
commercial dietary supplements. This method demonstrates
the ability of the PinAAcle 900T flame atomic absorption
system to accurately measure minerals in both commercial
tablets and food simulation diets. It is an efficacious method
that allows for cost effectiveness and ease of use, with
less operator training than other analytical methods. The
PinAAcle 900H (Flame and Deuterium Furnace) and PinAAcle
900F (Flame only) spectrometers can also be used for this
application.

0.03

K	

Conclusions

0.003

PerkinElmer, Inc.
940 Winter Street
Waltham, MA 02451 USA	
P: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com

For a complete listing of our global offices, visit www.perkinelmer.com/ContactUs
Copyright ©2011, PerkinElmer, Inc. All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners.
009636A_01

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The Determination of Minerals and Metals in Multi-Mineral/Multi- Vitamin Tablets by Flame Atomic Absorption Spectroscopy

  • 1. a p p l i c at i o n N o t e Atomic Absorption Authors: Lee Davidowski, Ph.D. Lorraine Foglio PerkinElmer, Inc. Shelton, CT 06484 USA The Determination of Minerals and Metals in Multi-Mineral/MultiVitamin Tablets by Flame Atomic Absorption Spectroscopy Introduction There are many mineral dietary supplements available in today’s marketplace to ensure that mineral deficiencies do not occur in one’s diet. The mineral content of these products must be verified for quality control (QC) purposes. Furthermore, the Nutritional Labeling and Education Act of 1990 mandates accurate labeling of all food supplements sold in the U.S. which means accurate testing of the products is mandatory. In many labs, this task is accomplished by the technique of flame atomic absorption spectroscopy (FAAS). FAAS has the advantages of lower initial cost, low cost per analysis, and requires less operator training than many other trace elemental techniques. The objective of this work is to demonstrate the applicability of FAAS using the PerkinElmer® PinAAcle™ 900T to accomplish this task. Seven elements are determined in two commercially available multi-mineral tablets, a NIST® Standard Reference Material, and a commercial reference material which simulates a mixed food diet.
  • 2. Experimental Instrumentation The PinAAcle 900T flame and longitudinal Zeeman furnace atomic absorption spectrometer controlled by WinLab32™ for AA software, running under Microsoft® Windows® 7, was used for all analyses (PerkinElmer, Inc., Shelton, CT). A high-sensitivity nebulizer (Part No. N3160112) with a spacer was employed. Single-element Lumina™ hollow cathode lamps (HCLs) were used and the instrumental operating conditions for each element in this application are shown in Table 1. A four-second integration time and three replicates were used for all elements. approximately one hour and warmed, not to boiling, on a hot plate. Deionized water was then added to the volumetric mark after removal of the magnetic stir bar. The sample digestion solution was then filtered through Whatman® 46 paper (passes < 8 micron) to remove waxy undissolved material, presumably from the tablet’s coating. The filtrate was then analyzed, after appropriate dilution, against singleelement aqueous standards (PerkinElmer Pure) for elemental quantitation. A Certified Reference Material Mixed Food Diet (CRM-MFD) (High Purity Standards, Charleston, SC) was prepared by dissolution, following the manufacturer’s instructions, to an appropriate concentration for individual elements. All tablets also contained about 2 mg/tablet of silicon, much of which may have remained undissolved. For an accurate measurement of the silicon, HF (trace metal grade) and plastic volumetric flasks should be employed for the dissolution. For calcium and magnesium determinations, La(NO3)2 (reagent grade) was added to all standards, blank and samples to a concentration level of 0.2% to remove chemical inferences from other matrix elements. For potassium determinations, CsCl (reagent grade) was added to all test solutions to a concentration level of 0.2% as an ionization buffer. Figure 1. PinAAcle 900T atomic absorption spectrometer. Results Sample and Standard Preparation One NIST® SRM 3280 Multi-vitamin/Multi-mineral Tablet and two over the counter multi-vitamin/multi-mineral tablets were coarsely ground. Nominally, 0.75 g were weighed out and rinsed into a 1000 mL volumetric flask containing about 20 mL of ASTM® Type I deionized water (>16MΩ • cm). Four mL of HCl (trace metal grade), two mL of HNO3 (trace metal grade), and a magnetic stirring bar were then added to the flask. This sample digestion solution was stirred for All elements showed acceptable calibration criteria. The results obtained for the FAAS analyses of the multi-vitamin/ multi-mineral tablets are shown in Table 2. The values are corrected for laboratory sample dissolution steps and dilutions. The commercial tablets were calculated and reported in mg/ tablet as this was the unit shown and guaranteed on each label. All elements were found to be within the certified range for the NIST® 3280 tablet. Both commercial tablets showed good correlation to labeled quantity guaranteed by the manufacturer. Table 1. PinAAcle 900T Instrumental Parameters. Element Parameter Ca Mg K Fe Zn Cu Mn Wavelength (nm) 422.7 285.2 766.5 248.3 213.9 324.8 279.5 Slit Width (nm) 0.7 0.7 0.7 0.2 0.7 0.7 0.2 Oxidant Flow (L/min) 10 10 10 10 10 8.7 10 C2H2 Flow (L/min) 2.5 2.5 2.2 2.5 2.0 2.5 5 1 4 4 1 4 2 HCL Part Nos. N3050114 N3050144 N3050139 N3050126 N3050191 N3050121 N3050145 Standard Part Nos. 2 2.5 Working Range (mg/L) N9303763 N9300179 N9303779 N9303771 N9300178 N9300183 N9303783
  • 3. Table 2. Corrected FAAS results for one certified reference material and two commercial multi-vitamin/multi-mineral samples. Element NIST® 3280 (mg/g) Certified Found Commercial Tablet 1 (mg/Tab) SD Label Found SD Commercial Tablet 2 (mg/Tab) Label Found SD Ca 110.7 107 0.8 162 163 0.6 200 211 0.6 Mg 67.8 69.1 0.2 100 107 0.4 100 109 0.4 K 53.1 53.8 0.3 80 83.8 0.4 80 90.7 0.4 Fe 12.35 12.9 0.05 18 19.1 0.08 n/a 0.23 0.006 Zn 10.15 10.1 0.02 15 15.5 0.04 15 15.2 0.03 Cu 1.4 1.42 0.01 2 2.19 0.01 2 2.04 0.01 Mn 1.44 1.48 0.01 2 1.91 0.01 2 2.04 0.01 The results for the FAAS analysis of the Certified Reference Material – Mixed Food Diet from High Purity Standards – are given in Table 3. All elements were found to be within 5% of the certified value, showing excellent agreement with the reference material. Table 3. Mixed Food Diet CRM results using aqueous standards and FAAS on a PinAAcle 900T. CRM-MFD (mg/L) Element Certified Found SD Ca 40 39.8 0.2 Mg 12 11.8 160 159 0.005 Fe 0.8 0.802 0.005 Zn 0.3 0.290 0.001 Cu 0.06 0.061 0.001 Mn 0.2 0.191 The mineral content of multi-vitamin/multi-mineral tablets must be determined in order to ensure the quality of commercial dietary supplements. This method demonstrates the ability of the PinAAcle 900T flame atomic absorption system to accurately measure minerals in both commercial tablets and food simulation diets. It is an efficacious method that allows for cost effectiveness and ease of use, with less operator training than other analytical methods. The PinAAcle 900H (Flame and Deuterium Furnace) and PinAAcle 900F (Flame only) spectrometers can also be used for this application. 0.03 K Conclusions 0.003 PerkinElmer, Inc. 940 Winter Street Waltham, MA 02451 USA P: (800) 762-4000 or (+1) 203-925-4602 www.perkinelmer.com For a complete listing of our global offices, visit www.perkinelmer.com/ContactUs Copyright ©2011, PerkinElmer, Inc. All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners. 009636A_01