Determination of Nutrition Labeling Education Act

Minerals in Foods by Inductively Coupled Plasma-

Optical Emission Spectroscopy
Karen W. Barnes* and Ebenezer Debrah
The Perkin-Elmer Corporation
761 Main Avenue, Norwalk, CT 06859-0215 USA

INTRODUCTION provisions of the Federal Food,

ABSTRACT Drug, and Cosmetic Act and
In the past, the analysis of metals requires full nutritional labeling for
The Nutrition Labeling in foods was performed by food
Education Act of 1990 (NLEA) most Food and Drug Administration
manufacturers primarily to ensure (FDA) regulated packaged food
mandates significant reform of product quality or safety. Nutrient
food labels and requires exten- products. Very few products are
labeling was required on a food exempt from NLEA. The complete
sive chemical testing and analyti-
product only if health claims were regulations have been published (2)
cal method development to
implement. Many minerals and made or implied on the food label and a May 8, 1994 compliance
nutrient metals are targeted for (1). Regulatory agencies typically deadline was established. There are
labeling. Part of the analytical performed metal or mineral analysis 14 mandatory nutrients including
challenge to be met results from to determine nutrient content, to calcium, iron, and sodium. Thirty-
the large numbers of samples to confirm or establish product iden- four other nutrients, including nine
be tested and widely divergent tity, to determine compliance with
levels of the elements of interest additional metals, may be labeled
current trade and food labeling voluntarily. The mandatory and
within the samples. Ideally, the laws, and to ensure product safety.
new methodology developed for voluntary nutrients are listed in
In an attempt to assist consumers in Table I. It has been predicted that
food analysis will be generic and
maintaining healthy dietary prac- the voluntary nutrients will become
applicable to many elements and
matrices simultaneously. tices, the United States Congress mandatory at some point in the
enacted the Nutrition Labeling and future (3). It has been estimated
This work discusses an Induc- Education Act of 1990 (NLEA) on that 17000 food companies in the
tively Coupled Plasma-Optical November 8, 1990. NLEA amended United States are affected by NLEA,
Emission Spectroscopy (ICP-OES)
method for the determination
of nutrient metals and minerals
TABLE I
in juice, corn products, milk, The Nutrition Labeling Education Act of 1990
and ice cream. Sample prepara- Food Labeling Requirements
tion time was the primary limita- Mandatory Voluntary
tion to sample throughput and nutrients nutrients
this was minimized using micro-
wave digestion. Due to the wide Calories Calories from saturated fat Vitamin K Cu
linear dynamic range of the ICP- Calories from fat Calories from unsaturated fat Thiamin Mn
OES, trace and macro levels of
nutrients were determined simul-
Total fat Calories from carbohydrates Riboflavin Fluoride
taneously in samples without Saturated fat Calories from protein Niacin Cr
multiple dilution/analysis itera- Cholesterol Unsaturated fat Vitamin B6 Mo
tions. Quality assurance (QA) was
performed by analyzing replicate Sodium Polyunsaturated fat Folate Chloride
samples, fortifying and analyzing Total carbo-
samples and reagent blanks, and hydrates Monounsaturated fat Vitamin B12
analyzing Standard Reference
Materials. Acceptable precisions, Total sugars Sugar alcohols Biotin
spike recoveries and agreement Dietary fiber Soluble fiber Pantothenic Acid
with authentic values and certi- Protein Insoluble fiber Phosphorus
fied values were obtained.
Vitamin A Protein as % Magnesium
Vitamin C Potassium Zinc
Calcium Vitamin D Iodine
*Corresponding author.
Iron Vitamin E Selenium

Atomic Spectroscopy 18 (2), pp 41-54, March/April 1997. Copyright © 1997 by the Perkin-Elmer Corp. All rights reserved.
that labels for 196 000 to 257 000 based on relative fat, carbohydrate, neously monitor trace levels of
products will require modification, and protein content. AOAC elements in the presence of macro
and that industry costs to proposes that a method can be levels of other elements. ICP-OES
implement the labeling laws will tested for all food matrices by ana- features multielement capability,
approximate $2 billion (4). lyzing eighteen types of samples, wide linear dynamic range, high
two from each sector of the food analytical sensitivity, and high sam-
The analysis of metals and miner- triangle. The food matrix triangle ple throughput. All these are attrib-
als in foods is challenging due to is presented in Figure 1 and is utes that will prove invaluable to
the wide range of concentrations reprinted with permission from analysts striving to meet the chal-
present, which may vary from ppb The Referee, Volume 17, Number 7, lenges posed by NLEA.
(ng/mL) to percent levels. The situ- pages 06-07, Copyright 1993 by
ation is further complicated by nat- Extensive sample preparation of
AOAC International.
urally occurring seasonal and foods before elemental analysis is
varietal differences. The use of offi- The FDA will regulate based common and in most cases proves
cial validated analytical methodol- upon a 20% tolerance of label to be more time-consuming than
ogy is preferred by regulatory claim (2) and state regulatory agen- the actual analysis. Methods involv-
agencies; however, many official cies will probably adopt similar ing hot plate digestion in open ves-
methods are analyte and matrix spe- guidelines for monitoring compli- sels or dry ashing followed by acid
cific. A review of current validated ance. Although no AOAC food dissolution are often employed, but
Association of Official Analytical methods currently employ Induc- are time-consuming and prone to
Chemists International (AOAC) tively Coupled Plasma-Optical Emis- contamination and evaporative
methodologies for minerals and sion Spectroscopy (ICP-OES), it is losses. Microwave digestion has
metals in foods (5) revealed that a well-established multielement been shown to be an acceptable
many single element methods are technique, and the analysis of foods alternative and has been success-
currently in use. These methods has been a natural application (9). fully applied to food analyses (10).
employ the techniques of colorime- Due to the wide variations of min-
This paper discusses a simul-
try, UV/Visible spectrophotometry, eral levels in foods, a multielement
taneous ICP-OES analysis with
and flame and graphite furnace technique must be able to simulta-
atomic absorption spectrophotome-
try. Many of the methods have sam-
ple throughput constraints and
relatively narrow linear dynamic
ranges, and others require the use
of solvents banned by the Montreal
Protocol on Substances that
Deplete the Ozone Layer (6).
A collaborative study was per-
formed for metals in foodstuffs by
dry ashing followed by atomic
absorption spectrophotometry (7);
however, NLEA elements were not
specifically targeted. Neither the
methodology from the collaborative
study nor existing official methods
can be used to simultaneously
determine all the elements speci-
fied in NLEA. Time constraints
make multiple sample dilutions
and independent analysis impracti-
cal and limit the utility of some vali-
dated methods. AOAC recognized
the need for improved methodol-
ogy and developed a tool to help
analysts develop rugged, generic
methods. The food triangle (8)
categorizes foods into nine sectors Fig. 1. The food matrix triangle.

2

microwave digestion procedures
for the determination of the NLEA
specified metals and minerals in
food. Products were chosen from
sectors 2, 5, 6, and 7 of the food
triangle. Juice, corn, and grits are
found in sector 5. Whole milk lies
in sector 6, skim milk and lowfat
milk fall in sector 7, and ice cream
and chocolate belong in sector 2.
Peanuts that fall in sector 3 were
an ingredient in one of the ice
cream samples.
Although this study targets
NLEA elements, all the procedures
discussed here have been success-
fully used to analyze numerous tar-
get metals in different food or plant
matrices (K.W. Barnes unpublished
work, Bureau of Food Laboratory,
Florida Department of Agriculture
and Consumer Services, 1989-
1993). With the careful selection
of metallic analytes, many different
analytical questions may be
answered. For example, adulter-
ation and misbranding may be iden-
tified from metal profiles because
an adulterated product that has had
a valuable constituent abstracted
will often have a different metal
profile than an authentic product.
This is most useful as part of a
matrix of analytical tests. The geo-
graphical origin of a food or plant
may be determined by characteriz-
ing a metal fingerprint in a product
and comparing it with the finger-
print from a known, authentic
sample of the product. Related
cases of food tampering have been
linked by comparison of metal pro-
files. Metal analysis is appropriate
for the determination of food safety
as well. Food contamination with
lead from solders or aluminum from
breached can linings may be identi-
fied by analyzing the contaminated
product. Typically, the suspect
products are measured simultane-
ously with known, authentic prod-
ucts for comparison.
EXPERIMENTAL
Reagents
HNO3-Reagent Grade (Fisher Sci-
entific, Fair Lawn, NJ USA).
H2O2-30% Reagent Grade (J.T.
Baker, Phillipsburg, NJ USA).
Micro Laboratory Cleaner (Inter-
national Products Corporation,
Trenton, NJ USA).
HNO3-Double Subboiling
Distilled in Quartz (Seastar Chemi-
cals, Seattle, WA USA).
HCl-Double Subboiling Distilled
in Quartz (Seastar Chemicals, Seat-
tle, WA USA).
H2SO4-Double Subboiling
Distilled in Quartz (Seastar Chemi-
cals, Seattle, WA USA).
Standards-PE Pure™ Single Ele-
ment Standards (The Perkin-Elmer
Corporation, Norwalk, CT USA).
Distilled, deionized water,
18 MΩ, (Continental Water
Systems, San Antonio, TX USA).
Standard Reference Material
#1572 Citrus Leaves (National Insti-
tute of Standards and Technology,
Gaithersburg, MD USA).
Standard Reference Material
#1549 Milk Powder (National Insti-
tute of Standards and Technology,
Gaithersburg, MD USA).
Apparatus
Optima 3000™ Inductively Cou-
pled Plasma Optical Emission Spec-
trometer (Perkin-Elmer, Norwalk,
CT USA).
AS 90 Autosampler (Perkin-
Elmer, Norwalk, CT USA).
MDS 2100 microwave oven
(CEM, Matthews, NC USA)
Capping Station (CEM,
Matthews, NC USA).
Teflon® PFA microwave vessels
rated to 120 psig (CEM, Matthews,
NC USA).
3
Vol. 18(2), March/April 1997
Lined digestion vessels rated to
200 psig (CEM, Matthews, NC
USA).
Food processor designed for
home use.
High density polyethylene bot-
tles, Nalgene® or equivalent (Nalge
Company, Rochester, NY USA).
Instrumental
A CEM MDS 2100 microwave
with 950 watts power with temper-
ature and pressure monitoring and
control was used to digest all the
samples. The microwave was cali-
brated following the United States
Environmental Protection Agency
(EPA) calibration procedure that
involves heating a known volume
of water at specific powers (11).
The heaviest, most reactive sample
was used for temperature and pres-
sure monitoring in each group of
samples. The digestion programs
presented are recommended for
twelve samples. Fewer samples
require reducing the microwave
power or substituting vessels filled
with equivalent volumes of water
to compensate for the missing sam-
ples. Personal experience dictates
that the sample weights should be
kept at or below the recommended
weights to minimize the potential
for over-pressuring and venting dur-
ing the microwave digestion
process. Samples containing high
levels of sugars are apt to react
more quickly and to generate more
pressure. If these products are sub-
stituted for the materials analyzed
in this work, using smaller sample
sizes and lower powers are strongly
recommended to prevent over-pres-
suring.
The ICP-OES analyses were per-
formed on the Perkin-Elmer Optima
3000™ Inductively Coupled
Plasma-Optical Emission Spectrome-
ter equipped with a standard torch,
Scott-type spray chamber, and a
GemTip™cross-flow nebulizer. A
Perkin-Elmer® AS 90 Autosampler
featuring a quartz sample probe to
minimize sample cross contamina-
tion was used. The Optima 3000 is
a simultaneous ICP-OES instrument
with an echelle polychromator and
a segmented array charge-coupled
detector (SCD). Because measure-
ment of background and analyte
emissions occurs simultaneously,
accurate correction of transient
background fluctuations for multi-
ple lines for each element of inter-
est is possible. Also, due to the
simultaneous measurement, no
reduction in sample throughput
occurs from making measurements
at multiple wavelengths of an ele-
ment. Therefore, where possible,
multiple emission lines were mea-
sured simultaneously for each ele-
ment to verify analytical results.
Plasma conditions used for this
work are listed in Table II. No
attempt was made to optimize
source conditions for specific
analytes, rinse or read delays, or
to maximize sample throughput.
The analysis of different types of
TABLE II
Instrument Conditions for
the Optima 3000 ICP-OES
Parameter Setting
RF Power 1100 W
Nebulizer Flow 0.950 L/min
Auxiliary Flow 1.0 L/min
Plasma Flow 15 L/min
Sample Flow 1.0 mL/min
Source equilibration
time 15 s
Viewing Height 15 mm
Background Manual
correction selection of points
Measurement
processing mode Area
Auto
integration 1 s min–50 s max
Read delay 45 s
Rinse delay 45 s
Number of replicates 3 alent volume of dd H2O was added
samples was performed on different
days and because each sample
was in a different acid matrix,
optimum background correction
points (BGC) and peak windows
were determined as a function
of sample before the analysis was
performed. The standard concentra-
tions were matched to the antici-
pated levels in the diluted samples.
Sample Preparation
General Sample Preparation
All labware, except the high
density polyethylene (HDPE) bot-
tles used to store the diluted sam-
ples, was washed with Micro
laboratory cleaner, rinsed with
18 MΩ distilled, deionized water
(dd H2O), soaked in 30% (v/v)
reagent grade HNO3 and rinsed
with dd H2O. To minimize the
potential for contamination, dis-
posable powder-free gloves that
had been dipped in 30% (v/v)
reagent grade HNO3 were worn
throughout the entire sampling
process. Wolnik et al. (12) empha-
size the need for procedures to
control the analytical blank and
ensure sample integrity for success-
ful trace metal analysis.
Each food matrix required
different sample preparation tech-
niques, so each will be discussed
independently below; however,
a general sample preparation pro-
tocol was followed throughout the
experiment. Four subsamples were
prepared and analyzed for each
food sample. Standards, blanks,
spiked blanks, and wash solutions
were matrix-matched using acids
digested in the microwave as part
of the sample preparation proce-
dure. Water was added to the ves-
sels containing the acids for the
blank, standard, and fortified blank
to compensate for the lack of sam-
ple moisture before digestion. If
dry samples were digested simulta-
neously with wet samples, an equiv-
to the sample to compensate for
the missing sample moisture before
4
digestion. A concentrated stock
standard solution was used to pre-
pare a working standard and to for-
tify (spike) the blank and samples.
The samples and blanks were forti-
fied at levels that were anticipated
in the diluted samples, and spiked
samples and blanks were subjected
to digestion concurrently with the
samples to monitor any losses in
the microwave. Where possible,
Standard Reference Materials (SRM)
were obtained from the National
Institute of Standards and Technol-
ogy (NIST) for comparison with the
samples. The SRM materials were
also subsampled in quadruplicate
and subjected to microwave diges-
tion simultaneously with the samples.
Juice Sample Preparation
Single serving containers of
ready-to-drink juices were used for
this study. One container each of
Florida orange juice, Florida grape-
fruit juice, cranberry juice cocktail,
apple-cranberry juice cocktail, and
orange-strawberry-banana juice bev-
erage were sampled in quadrupli-
cate for this study. Each juice was
well shaken, opened and subsam-
pled by pouring directly from the
original containers into the
microwave vessels to minimize the
potential for contamination. Cran-
berry juice cocktail was selected as
the matrix to be spiked to monitor
recoveries. Clear, colored solutions
resulted for all samples using the
following digestion procedure mod-
ified from the CEM application note
for Fruit Juice and Pulp (13).
Digestion Procedure
Step 1: Accurately weigh ≤ 10 g
single-strength juice into the Teflon
PFA digestion vessels.
Note: Juice concentrates
with high Brix values require
smaller sample sizes to prevent
over-pressuring in the microwave.
Step 2: Add 10 mL concentrated,
ultrapure HNO3 and 2 mL concen-
trated, ultrapure H2SO4 to the
sample.

Step 3: Cap the vessel in the
capping station.
Step 4: Digest following the
Procedure Juice 1 in Table III.
Step 5: Cool for approximately
five minutes and vent vessels.
Step 6: Repeat Step 4 for juices
containing pulp.
Step 7: Cool for five minutes,
vent, and open the vessels using
the capping station.
Step 8: Add 3 mL 30% H2O2 to
the samples.
Step 9: After effervescence
subsides, transfer the samples
into clean, acid-washed volumetric
flasks and dilute to 100 mL with
dd H2O.
Step 10: Transfer the samples
to clean HDPE bottles.
Corn Products Sample Preparation
One 16 oz can of whole kernel
yellow sweet corn with liquid, one
16 oz can of 50% low salt golden
sweet corn with liquid, and one
24-oz box of white hominy grits
were purchased for this study. One
sample of pre-homogenized corn
was received from a vegetable man-
ufacturer. There was high potential
for product contamination from
opening the cans, so to minimize
the risk, each can was thoroughly
rinsed with dd H2O and dried with
a lint-free towel before opening. An
acid rinse was not used because of
the possibility of increased contami-
TABLE III
Microwave Digestion Program for Juice Analysis
Parameter Stage 1 Stage 2 Stage 3 Stage 4 Stage 5
Power (%) 10 20
Power (watts) 51
Pressure (psig) 20
Run time (min) 2 5
Time at parameter (min) 2 5
Fan speed (% of maximum) 100
nation by dissolving the can. The
cans were opened with a hand-held
can opener that had been washed
with Micro cleaner and rinsed with
dd H2O. All can contents, corn and
packing liquid, were homogenized
by processing in a small food
processor designed for home use.
The food processor was washed
with Micro cleaner and rinsed with
dd H2O before use and between
all samples. Acid was not used to
clean the food processor because
of the increased contamination that
would result from partial dissolu-
tion of the metal blade. Wolnik et
al. (12) reported using a food
processor with all plastic parts
presumably to prevent sample
contamination during grinding.
This was not an option for this
study although the metal blade in
the food processor was considered
a possible source of contamination
to the corn. The results indicate,
however, that no contamination
occurred. The samples were
processed for approximately two
minutes each until no further
reduction in particle size was appar-
ent. Thick, in-homogeneous slurries
resulted. The slurries were trans-
ferred into HDPE bottles for sub-
sampling. Each corn slurry was
well shaken before sampling from
the HDPE bottle, and the slurry
was poured directly into the
microwave vessels. No grinding
was performed on the grits. The
container of grits was well shaken
between samplings and the grits
0 15 0 Step 5: Cool for five minutes,
141 0 96 0 vent, and open the vessels.
50 20 80 0 Step 6: Add 2 mL of
2 15 5 the samples.
2 15 5 Step 7: Recap the vessels.
100 100 100 100
5
Vol. 18(2), March/April 1997
were removed directly from the
box by tapping into the microwave
vessels. SRM Corn has become
available from NIST, but was not
available when this work was per-
formed. Hence, a sample of NIST
SRM 1572 Citrus Leaves was sub-
stituted for the SRM Corn and
digested with the corn and grits
to provide additional quality assur-
ance. The whole kernel yellow
sweet corn with liquid was selected
for spiking to monitor recoveries.
Clear, colored solutions resulted
for all corn and grits samples from
the digestion procedure presented
below that was modified from the
CEM application note for Feed
Grain (14). The SRM Citrus Leaves
were not completely digested by
the process. Since the SRM was
not an accurate representation of
the corn matrix, no further diges-
tion was performed. The incompletely
dissolved citrus leaves samples
were allowed to stand in the sam-
ple tubes for approximately 20 min-
utes before ICP-OES analysis to
allow settling of the particulate
material. Sampling was performed
above the particulate layer. No
clogging of the sample probe,
nebulizer tubing, or nebulizer
resulted from the process.
Digestion Procedure
Step 1: Accurately weigh ≤ 2.0 g
grits and homogenized corn, or
< 0.8 g citrus leaves into the lined
digestion vessels.
Step 2: Add 10 mL concentrated,
ultrapure HNO3 to the samples.
Step 3: Cap the vessels.
Step 4: Digest following the
procedure Corn Part 1 in Table IV.
concentrated, ultrapure HCl to
 Step 8: Digest following the
procedure Corn Part 2 in Table V.
Step 9: Cool for five minutes,
vent, and open the vessels.
Step 10: Transfer the samples
into clean, acid washed volumetric
flasks and dilute to 100 mL with
dd H2O.
Step 11: Transfer the samples
to clean HDPE bottles.
Dairy Products Sample
Preparation
One half-pint (236 mL) container
of whole milk, 2% lowfat milk, and
two containers of skim milk with
the same "sell by" date from one
manufacturer were purchased and
sampled. The replicate containers
were sampled to give an indication
of sample-to-sample variation
within a product. This was deemed
necessary because identical date
codes may be used for multiple
lots of dairy products. Pint contain-
ers of premium high-fat, nonhomo-
geneous ice cream from various
manufacturers were purchased for
this study. Samples included vanilla
bean, chocolate, vanilla with choco-
late toffee bits, and a specialty ice
cream product with chocolate,
peanuts, rice, and peanut-butter-
flavored ice cream. The milk sam-
ples were shaken by hand and were
poured directly into the microwave
vessels from the original cartons.
Subsamples of each ice cream were
transferred into HDPE bottles,
allowed to fully melt, and shaken
by hand before sampling into the
microwave digestion vessels. One
of the skim milk samples and the
vanilla bean ice cream were
selected for fortification. NIST SRM
1549 Milk Powder was digested
with the milk and ice cream sam-
ples. All samples were subjected to
the first digestion step without the
cap (see Table VI) to remove easily
oxidized materials and to prevent
over-pressuring of the samples after
the addition of the acid (Personal
communication with Sara Littau,
CEM Corporation, 1993). Clear yel-
low solutions resulted for all sam-
ples following the procedure
modified from the CEM application
note for Infant Formula (15). Some
residual fat was found in the spiked
ice cream because the acid was
diluted by the stock spiking solu-
tion. Since the other samples had
been completely digested and
because it was considered unlikely
that the fat would bind metals in a
strong acid matrix, the solution was
decanted and analyzed without
additional digestion. The ice cream
spike recoveries indicate that this
was an acceptable compromise.
The digestions of milk and ice
cream were performed on different
days, so full quality assurance (QA)
was run with each digestion
process and included spiked
blanks, spiked samples, and four
subsamples of the SRM.
Digestion Procedure
Step 1: Accurately weigh < 6 g
liquid milk, < 0.75 g powdered
milk, or < 1.75 g ice cream into
Teflon PFA microwave vessels.
Note: Milk products
with high sugar contents such as
instant cocoa mix, diet meals,
and liquid chocolate milk require
smaller sample sizes to prevent
over-pressuring in the microwave.
Step 2: Digest the samples
uncapped following the
Procedure Ice Cream 1 in Table
VI.
Step 3: Add 15 mL
concentrated, ultrapure HNO3 to
each sample.
Step 4: Cap the vessels in the
capping station.
Step 5: Digest the samples fol-
lowing the Procedure Ice Cream 2
in Table VII.
Step 6: Cool for five minutes
and vent the vessels.
Step 7: Digest the samples fol-
lowing the Procedure Ice Cream 3
in Table VIII.
Step 8: Cool for five minutes,
vent, and open the vessels using
the capping station.

TABLE IV TABLE V
Microwave Digestion Program Microwave Digestion Program
for Corn Analysis – Part 1 for Corn Analysis – Part 2
Parameter Stage 1 Stage 2 Stage 3 Stage 4 Stage 5 Parameter Stage 1 Stage 2 Stage 3
Power (%) 10 45 45 45 45 Power (%) 10 50 0
Power (watts) 51 366 366 366 366 Power (watts) 51 411 0
Pressure (psig) 20 40 80 120 160 Pressure (psig) 20 90 20
Run time (min) 2 10 10 10 20 Run time (min) 2 15 5
Time at parameter Time at parameter
(min) 2 5 5 5 10 (min) 2 5 5
Temperature (*C) 0 75 85 100 120 Temperature (*C) 20 90 0
Fan speed Fan speed
(% of maximum) 100 100 100 100 100 (% of maximum) 100 100 100

6
 Vol. 18(2), March/April 1997

Step 9: Add 2 mL of 30% H2O2 to
each sample and allow the efferves-
cence to stop.
Step 10: Cap the vessels in the
capping station.
Step 11: Digest the samples fol-
lowing the Procedure Ice Cream 4
in Table IX.
Step 12: Cool for five minutes,
vent, and open the vessels using the
capping station.
Step 13: Transfer the samples
into clean, acid washed volumetric
flasks and dilute to 100 mL with dd
H2O.
Step 14: Transfer the samples to
clean HDPE bottles.
RESULTS AND DISCUSSION
General
For ease of comparison, the
results obtained for this work are
presented with available authentic
data and calculated concentrations
based on available label claims.
Maximum values for claims
expressed as less than 2% of the
United States Recommended
Daily Allowance (USRDA) are
listed where applicable. Current
labeling laws were applied in the
calculations (1). All concentrations
for this work are expressed in
mg/mL (ppm). The mean value
obtained for the four subsamples
of each sample is reported in the
experimental column and the
reported uncertainty is one
standard deviation of the measure-
ment. Se, Cr, and Mo were not
detected in any juice, corn, grits,
milk, or ice cream samples. Wolnik
et al. (12) reported that the ICP-OES
detection limits for Pb, Cd, and Se
are not sufficient for routine deter-
mination of background levels in
crops and that Mo levels are near
the detection limit for ICP-OES.
Although the levels of Se, Cr, and
Mo in the foods were below the
detection limits for this work, the
analysis of these elements may be
possible with plasma optimization
and the implementation of precon-
centration techniques. Increasing
the sample size might be possible
in a microwave digestion system

TABLE VI TABLE VII

Microwave Digestion Program for Microwave Digestion Program for
Ice Cream Analysis – Part 1 Ice Cream Analysis – Part 2
Parameter Stage 1 Stage 2 Parameter Stage 1 Stage 2 Stage 3 Stage 4 Stage 5
Power (%) 10 64 Power (%) 10 64 35 0 64
Power (watts) 51 538 Power (watts) 51 538 276 0 538
Pressure (psig)a 20 20 Pressure (psig) 20 50 15 20 80
Run time (min) 0.01 1.50 Run time (min) 2 1.50 10 2 15
Time at parameter (min) 0.01 1.50 Time at parameter (min) 2 1.5 10 2 15
Temperature (*C) 0 0 Temperature (*C) 50 65 70 50 75
Fan speed Fan speed
(% of maximum) 100 100 (% of maximum) 100 100 100 100 100
a Digestion was performed with microwave vessels
uncapped, so pressure setting was arbitrary.

TABLE VIII TABLE IX

Microwave Digestion Program for Microwave Digestion Program for
Ice Cream Analysis – Part 3 Ice Cream Analysis – Part 4
Parameter Stage 1 Stage 2 Stage 3 Stage 4 Stage 5 Parameter Stage 1 Stage 2 Stage 3
Power (%) 10 71 0 78 0 Power (%) 0 71 0
Power (watts) 51 601 0 663 0 Power (watts) 0 601 0
Pressure (psig) 10 85 20 85 0 Pressure (psig) 20 85 20
Run time (min) 1 15 5 15 5 Run time (min) 5 10 5
Time at parameter (min) 1 15 5 15 5 Time at parameter (min) 5 10 5
Temperature (*C) 85 85 0 90 80 Temperature (*C) 0 85 0
Fan speed Fan speed
(% of maximum) 100 100 100 100 100 (% of maximum) 100 100 100

7
usable to higher pressures. Ultra-
sonic nebulizers, that typically
give an order of magnitude
improvement in detection limits
over conventional pneumatic nebu-
lizers, would offer additional sensi-
tivity. A systematic combination of
all of the above would be recom-
mended. Sample throughput for the
study was impressive, even though
throughput optimization was not
performed. The determination of
31 analytical lines in triplicate for
a sample of grits was performed in
180 seconds for elements ranging
from percent to µg/mL (ppm) lev-
els. Ninety seconds of read and
rinse delay overhead were included
in this time, so the actual analysis
was performed in 90 seconds. Sam-
ple throughput could be improved
by optimizing read and rinse delays
and by increasing the sample intro-
duction rate and the rate at which
the sample is introduced into the
plasma. For laboratories with large
sample loads, optimization of sam-
ple throughput will be necessary.
Considering that FDA will regu-
late compliance with NLEA based
upon a ±20% criteria, the protocols
employed to prevent outside conta-
mination may be excessive and
time-consuming; however, each
process discussed is appropriate for
monitoring metals for any of the
reasons discussed in the introduc-
tion. In which case, the ±20% crite-
ria may not be appropriate and
contamination could be an impor-
tant consideration.
Juice
Orange Juice
The label claimed that the
juice was 100% pure Florida orange
juice. Values obtained for this work
compare favorably with average
values reported in RSK (16) and
Afnor Fruit Juice Specifications
(17) and with the results presented
by McHard (18) for a juice from
Florida or possibly Brazil. Complete
differentiation could not be made
with the suite of elements analyzed;
however, the juice does not appear
to be of Californian or Mexican ori-
gin. McHard's work for Florida
orange juice, based on dry ashing,
has been included with the experi-
mental data in Table X.
Grapefruit Juice
Results for this work compare
favorably with authentic data and
were consistent with Na claims on
the product label. This juice was
reconstituted, so Ca, Mg and Na lev-
els reflect the properties of the
water used during processing. The
poor precision obtained for this
product may reflect the inhomo-
geneity due to the presence of pulp
in the sample. Afnor values in ppm
for grapefruit, USDA (19) reference
values for grapefruit juice diluted
from frozen concentrate, and label
claims are presented with the
experimental data in Table XI.
Fruit Beverage
This product was labeled Orange
Strawberry Banana juice beverage
and grape juice, high fructose corn
syrup, sucrose and sodium citrate
were claimed in the ingredient list.
The product was misbranded, a
term applied to false and misleading
labeling, because grape juice was
not specified in the name and it
was the second most predominant
juice present in the blend. From the
Ca and Mg results, the blend
appears to consist of approximately
50% juice. Due to the added citrate
salt, the Na results cannot be used
to determine authenticity of the
juice or to evaluate the analytical
results but would be required to
comply with NLEA. The poor preci-
sion for Fe (see Table XII) may be
attributed to sample contamination
from the laboratory environment.
A conclusion of loss due to the
microwave digestion process is
inconsistent with the results for
other juices and the spike recover-
ies. Authentic orange, strawberry,
grape, and banana data from USDA

TABLE X TABLE XI
ICP-OES Results for Orange Juice ICP-OES Results for Grapefruit Juice Compared with
Compared with Authentic Florida Orange Package Label Claims and Authentic Grapefruit Juice
Juice Reference Values in µg/mL Reference Values in µg/mL
Element Florida Orange Element USDA Afnor
wavelength Experimental Juice wavelength Experimental reference reference
Ca 396.845 85.3 ± 0.4 67–123 Ca 396.845 103.2 ± 0.6 80 50–240
Cu 224.702 0.43 ± 0.01 0.239–0.460 Cu 224.702 0.33 ± 0.02 0.33 ≤5
Fe 238.200 0.84 ± 0.01 0.641–5.58 Fe 238.200 0.79 ± 0.06 1.4 ≤ 15
K 766.515 1972 ± 10 1520–2660 K 766.515 1327 ± 4 1360 1100–2500
Mg 279.553 103.4 ± 0.3 95–140 Mg 279.553 88.3 ± 0.3 110 70–170
Na 589.589 8.64 ± 0.07 3–9 Na 589.589 23.36 ± 0.02 10 ≤ 40
P 177.436 206.4 ± 2.2 124–240 P 177.436 137.5 ± 1.3 140 125-180
Zn 206.198 0.4 ± 0.1 0.242–0.480 Zn 206.198 0.9 ± 0.2 0.5 ≤5

8
 Vol. 18(2), March/April 1997

TABLE XII
ICP-OES Results for the Mixed Fruit Beverage Compared with
USDA Authentic Juice and Fruit Reference Values in µg/mL
USDA USDA USDA USDA
Element Orange Grape Raw Raw
wavelength Experimental Juice Juice Strawberries Banana
Ca 396.845 55.4 ± 0.7 100 90 140 60
Cu 224.702 0.14 ± 0.03 0.4 0.28 0.49 1.04
Fe 238.200 0.61 ± 0.40 1.7 2.4 3.8 3.1
K 766.515 584.3 ± 7.3 1900 1320 1660 3960
Mg 279.553 41.6 ± 0.4 110 100 100 290
Na 589.589 23.40 ± 0.02 10 30 10 10
P 177.436 137.5 ± 1.3 110 110 190 200
Zn 206.198 0.9 ± 0.2 0.4 0.5 1.3 1.6

Fig. 2. Spike recoveries for juice
analysis.
(19), and experimental data for the
fruit beverage are presented in
Table XII.
Cranberry Juice Cocktail and
Apple Cranberry Juice Cocktail
Cranberry juice cocktails typi-
cally contain 25% pure cranberry
juice and apple-cranberry juice
blends typically contain 10% apple
and 15% cranberry juice (Personal
communication with Allan Brause,
Analytical Chemical Services of
Columbia, Inc. 1993). The results
obtained in this work are consistent
with blends of authentic juices and
with the label claims. USDA values
for bottled cranberry juice cocktail
(19) and apple juice values from
Afnor are presented with label val-
ues and the experimental data in
Table XIII.
Juice Spike Recoveries
Results are presented in Figure 2.
Recoveries ranged from a low of
96.1% for Mg to a high of 106.1%
TABLE XIII
ICP-OES Results for Cranberry Juice Cocktail and Apple Cranberry
Juice Cocktail Compared with Package Label Claims and USDA
Authentic Juice Reference Values in µg/mL
Apple Apple
Cranbery Juice Cocktail Cranberry Cranberry Apple
Element Juice Juiice Juice
wavelength Experimental Label USDA Experimental Label Afnor
Ca 396.845 31.8 ± 0.5 <115 30 30.0 ± 0.2 <79.1 30–120
Cu 224.702 0.04 ± 0.03 0.13 0.07 ± 0.01 ≤5
Fe 238.200 1.9 ± 0.1 <2.1 1.6 1.3 ± 0.1 < 1.4 ≤ 10
K 766.515 193.4 ± 1.5 240 261.8 ± 1.6 237 700–1500
Mg 279.553 10.6 ± 0.2 30 14.8 ± 0.2 40–80
Na 589.589 6.2 ± 0.2 57.5 40 20.0 ± 0.1 < 40 5–80
P 177.436 10.2 ± 0.2 10 21.4 ± 0.1 40–100
Zn 206.198 0.3 ± 0.2 0.2 0.3 ± 0.2 ≤5
for Se in the blank, and 97.7% for from the USDA (20) and calculated
Mg to 105.6 for Se in the juice. concentrations are based upon
available can label claims in Table
Corn Products XIV. Variations of 80–120% of label
claim are typical and will be
Corn and Grits
According to the supplier of the allowed by NLEA. Results for grits
are presented in Table XV and are
homogenized corn sample, corn is
one of the most popular vegetables compared with available authentic
data (21) and label claims. The
in the United States. Lead was
included in the suite of analytes for mean and standard deviation values
are for three samples of grits
this product because of the interest
in monitoring levels in children's because one sample was lost during
diets. The experimental values for the processing. Chromium, Mo,
metals obtained for corn are pre- Pb, and Se were not detected in
sented with available authentic data any corn or grits samples; however,

9
 TABLE XIV TABLE XV
ICP-OES Results for Corn Samples Compared with ICP-OES Resultsa for Enriched White
Package Label Claims and USDA Whole Kernel Corn Hominy Grits Compared with Pack-
Reference Values age Label Claims and USDA Refer-
in µg/mL ence Values in µg/mL
Element USDA Processora Low Salt Golden Sweet USDA Enriched White
wavelength Corn Sample Corn Corn White Hominy Hominy Grits
Found Label Found Label Grits Found Label
Ca 317.933 40 31.43±11.53 31.47±0.81 <162 21.28±1.22 <176 20 16.54±1.98 <714
Ca 393.366 40 32.09±11.29 32.19±3.88 <162 21.62±0.84 <176 20 17.49± 2.05 <714
Ca 396.847 40 31.89±11.06 31.94±3.88 <162 21.60±0.84 <176 20 17.41±2.09 <714
Cu 224.700 0.56 0.27±0.07 0.14±0.02 0.25±0.02 0.75 0.41±0.04
Cu 324.754 0.56 0.32±0.04 0.194±0.006 0.25±0.01 0.75 0.45±0.01
Fe 238.204 3.5 4.02±0.15 2.84±0.33 3 3.00±0.18 6 39.1 14.77±1.72 26
Fe 239.562 3.5 4.03±0.15 2.80±0.33 3 3.00±0.17 6 39.1 16.46±1.23 26
K 766.491 1530 1666±9 1541±18 1377 1260±7 1370 1679±57 1071
Mg 279.553 160 196.0±1.7 167.7±1.7 126.2±1.3 270 366.9±45.4
Mg 280.270 160 196.3±2.2 168.9±1.5 125.7±1.4 270 369.7±46.5
Mn 257.610 0.33 1.04±0.02 0.73±0.02 0.56±0.07 1.06 1.29±0.11
Mn 260.569 0.33 1.06±0.02 0.74± 0.02 0.56±0.07 1.06 1.32±0.11
Na 589.592 2530 2184±23 1575±24 1458 2473±37 3436 10 0.5±0.1 <179
P 177.428 510 575.5±18.9 479.3±11.8 486 373.4±6.5 730 1002±61
P 213.618 510 563.3±1.5 500.3±3.5 486 397.0±2.4 730 955.4±77.5
Zn 202.548 3.6 5.05±1.86 3.22±0.61 2.27±0.31 4.1 5.1±0.4
Zn 206.200 3.6 5.12±1.76 3.35±0.62 2.41±0.25 4.1 5.3±0.5
Zn 213.856 3.6 5.08±1.74 3.34±0.61 2.38±0.22 4.1 5.1±0.4
a
Pre-homogenized sample received from vegetable processor. a
Using same element wavelengths as in
Table XIV.

the spike recoveries were quite
good. The high relative standard
deviations seen for the corn and
grits samples (see Tables XIV and
XV) may be attributed to sample
in-homogeneity and could be
improved by more rigorous process-
ing of the samples. This claim is
based on similar conclusions drawn
by Wolnik et al. (12) who reported
higher % RSD values for corn than
for vegetables that were more easily
homogenized.
Corn Spike Recoveries
Spike recoveries are presented
in Figure 3. The recoveries indicate
that no gross contamination
occurred from the grinding process
with the metal blade. The high
recoveries for Ca and Zn found in
the corn may be attributed to sam-
ple in-homogeneity or to possible
contamination from slivers of the
can lid from opening the product.
The elevated values for Se may be
attributed to increased error of mea-
surements near the limit of detec-
tion.
NIST SRM 1572 Citrus Leaves
The results for the SRM Citrus
Leaves are presented in Table XVI.
The levels of Cr, Mo, and Se in the
diluted sample solutions were
below the limit of detection for
the determination. Due to the high
levels of Ca present in the citrus
leaves, quantification was not possi-
ble without additional dilution at
the two primary lines for the ele-
ment, 393.366 nm and 396.847 nm,
selected for the study. The use of
an additional line with a higher
background equivalent concentra-
tion (BEC) would have been prefer-
able. This was not deemed
necessary because the SRM was
a poor match for the corn and grits.
Reference values for Ca in corn and
grits are at 40 and 20 µg/g, respec-
tively. Calcium is present in the
SRM at 31,500 µg/g. The poor
recoveries for Fe (see Table XVI)
were anticipated based on Lajunen's
work (22) and may be attributed to
the incomplete digestion procedure.
Complexation with undissolved sili-
cates or selective sorption of Fe on
the surface of the insoluble plant

10
 Vol. 18(2), March/April 1997

material are possible explanations.
Although this SRM Citrus Leaves
were a poor substitution for the
corn SRM, the values obtained do
suggest that the micro-wave diges-
tion protocol used for this work is
applicable for many matrices with
different mineral levels.
Dairy Products
Milk and Ice Cream
For ease of comparison, the
experimental values obtained for
this work are presented with USDA
reference data (23) and label
claims. Only limited reference and
label information was available for
the ice cream samples. Chromium,
Mo, and Se were not detected
in any samples, and Cu was not
detected in any ice cream samples
although the spike recoveries
were acceptable for these elements.
Results for the milk samples are
presented in Tables XVII–XIX.
Good correlation was found
between the experimental results,
USDA reference values, and label
claims. Excellent agreement was
found for the two different cartons
of skim milk, indicating that this
method would be well suited for
routine use in a dairy quality labo-
ratory. Ice cream results are
presented in Tables XX–XXII.
Although USDA reference values
were not available for the specialty
ice cream product with chocolate,
peanuts, rice, and peanut-butter-
flavored ice cream or for the ice
cream with chocolate toffee bits,
some conclusions can be drawn
because there was satisfactory
sample-to-sample precision and
excellent agreement between wave-
lengths for the elements. The poor
precisions for some of the elements
may be attributed to sample inho-
mogeneity and could be improved
by more rigorous blending of the
samples. Excellent agreement was
found between the various lines
for both types of samples showing
that major and minor nutrients can
be measured simultaneously.
Milk and Ice Cream Spike
Recoveries
Reagent blanks and samples
of skim milk and vanilla bean ice
cream discussed in the previous
sections were spiked with the
elements of interest, processed
through the microwave procedure,
and analyzed with the regular
samples. The spike recoveries
are presented in Figures 4–5. The
recoveries indicate that no gross
contamination or losses occurred
during the sample preparation.
The poor results for Se are again
due to spiking at levels too near the

TABLE XVI
ICP-OES Results for NIST SRM1572 Citrus Leaves in µg/mL
Element NIST SRM 1572 Citrus Leaves
wavelength Certified Found
Ca 317.933 31500 ± 1000 30220 ± 774
Cu 224.700 16.5 ± 1.0 13.9 ± 0.5
Cu 324.754 16.5 ± 1.0 15.2 ± 0.6
Fe 238.204 90 ± 10 58.2 ± 2.6
Fe 239.562 90 ± 10 58.6 ± 2.7
K 766.491 18200 ± 600 18000 ± 806
Mg 279.553 5800 ± 300 5109 ± 308
Mg 280.270 5800 ± 300 5479 ± 176
Mn 257.610 23 ± 2 19.9 ± 0.7
Mn 260.569 23 ± 2 19.7 ± 0.6
Na 330.237 160 ± 20 140.1 ± 12.8
Na 589.592 160 ± 20 156.7 ± 5.9
P 177.428 1300 ± 200 1333 ± 72
P 213.618 1300 ± 200 1277 ± 33
Pb 216.999 13.3 ± 2.4 11.6 ± 0.9
Pb 220.353 13.3 ± 2.4 11.2 ± 0.3
Zn 206.200 29 ± 2 26.5 ± 0.6
Fig. 3. Spike recoveries for corn
analysis.

11
limit of detection. High spike recov-
eries for Fe in the spiked blank for
the ice cream analysis may be attrib-
uted to contamination from a failing
water purification system.
NIST SRM 1549 Milk Powder
The results for the SRM milk
powder analyses are presented in
Table XXIII and show the means
of the four subsamples digested
concurrently with the milk samples
and the four subsamples digested
with the ice cream samples. The
levels of Cr, Mo and Se in the sam-
ple solutions were below the limit
of detection for the determination
and are not reported. There was
excellent agreement with other
certified values.
CONCLUSION
This work demonstrates that
the analysis of metals and minerals
stipulated by NLEA in foods found
in sectors 2, 5, 6, and 7 of the food
triangle may be performed simulta-
neously using ICP-OES. This work
indicates that ICP-OES will be an
effective tool for the analysts
attempting to meet the challenges
imposed by NLEA. Microwave
digestion was shown to be an
effective sample preparation tool
allowing acceptable precisions,
spike recoveries, agreement
with SRM certified values, and
agreement with authentic values
were obtained for most samples
and elements. With the exception
of the citrus leaves containing
31.5% Ca, that could not be quanti-
fied due to the choice of analytical
lines, trace levels of elements were
determined simultaneously with
macro levels of nutrient metals
and minerals. Sample preparation
time, which was the primary
limitation to sample throughput,
was minimized due to the wide
liner dynamic range and the useful
analytical range of the ICP-OES.
All elements were determined
simultaneously in all samples,
except the citrus leaves, without
multiple dilution/analysis iterations.
Although no attempts were made
to optimize sample throughput,
actual instrumental sample through-
put was impressive relative to cur-
rent AOAC validated methods. If
rigorous optimization procedures
are implemented, then higher

TABLE XVII: ICP-OES Resultsa TABLE XVIII: ICP-OES Resultsa TABLE XIX: ICP-OES Resultsa
Whole Milk Compared 2% Lowfat Milk Compared Skim Milk Compared with
with Package Label Claims with Package Label Claims Package Label Claims and
and USDA Reference Values and USDA Reference Values USDA Reference Values
in µg/mL in µg/mL in µg/mL
USDA USDA USDA Skim Skim
Element Whole Whole Milk 2% Lowfat 2% Lowfat Milk Skim Milk 1 Milk 2
wavelength Milk Found Label Milk Found Label Milk Label Found Found
Ca 315.901 1190 1141±15 1271 1280 1205±11 1271 1230 1271 12254±1 1171±15
Ca 422.671 1190 1181±7 1271 1280 1241±8 1271 1230 1271 1202±12 1211±21
Cu 324.767 0.1 0.035±0.012 0.08 0.038±0.013 0.11 0.08±0.04 0.06±0.01
Fe 238.207 0.5 0.182±0.012 <1.5 0.5 0.18±0.01 <1.5 0.4 <1.5 0.33±0.07 0.49±0.09
Fe 239.568 0.5 0.182±0.017 <1.5 0.2 0.17±0.02 <1.5 0.4 <1.5 0.36±0.07 0.50±0.09
K 766.517 1520 1659±16 1620 1701±16 1660 1636±21 1593±17
Mg 279.089 130 112.8±1.1 140 117.6±1.2 110 116.2±1.2 112.7±1.6
Mg 279.563 130 114.8±0.7 140 119.3±1.1 110 118.2±0.7 112.8±1.2
Mg 280.283 130 114.5±0.8 140 119.1±1.1 110 117.6±0.7 113.0±1.2
Mn 257.614 0.04 0.023±0.002 0.02 0.024±0.002 0.02 0.0229±0.0001 0.031±0.005
Mn 260.573 0.04 0.024±0.002 0.02 0.025±0.002 0.02 0.025±0.001 0.032±0.005
Na 330.252 490 431.9±1.5 530 520 447.1±3.3 530 520 551 433.0±2.5 454.0±4.8
Na 589.596 490 443.9±3.3 530 520 464.2±5.9 530 520 551 435.8±4.7 462.3±8.4
P 177.441 930 924.7±10.9 1000 958.6±13.2 1010 925.6±14.9 948.2±17.3
P 213.625 930 928.2±11.9 1000 969.7±6.8 1010 953.3±10.3 946.4±15.4
P 214.914 930 918.5±12.7 1000 960.3±10.2 1010 955.6±11.2 949.0±12.0
Zn 206.200 3.8 3.94±0.10 4 4.23±0.09 4 4.24±0.09 4.29±0.08

a
Element wavelengths used in Table XVII also apply to Tables XVIII and XIX.

12
 Vol. 18(2), March/April 1997

TABLE XX: ICP-OES Resultsa TABLE XXI: ICP-OES Resultsa TABLE XXII: ICP-OES Resultsa
Vanilla Ice Cream Compared with Package Chocolate Ice Cream Specialty Ice Cream Product
Label Claims and USDA Reference Values Compared with Package and Ice Cream with
for Ice Cream with Different Fat Contents Label Claims Chocolate Toffee Bits
in µg/mL in µg/mL in µg/mL
USDA Specialty Vanilla with
Element Vanilla Ice Cream Ice Cream Chocolate Toffee
Wavelength (16% Fat) (10% Fat) Experimental Experimental Label Product Bits
Ca 315.901 1170 1280 1266±29 1180±41 1351 1490±19 1309±5
Ca 422.671 1170 1280 1280±33 1234±34 1351 1546±28 1340±18
Fe 238.207 0.5 0.9 0.50±0.03 8.4±0.3 4.9 3.2±0.2 2.7±0.7
Fe 239.568 0.5 0.9 0.50±0.05 8.3±0.3 4.9 3.3±0.2 2.7±0.7
K 766.517 1590 1990 1755±41.35 3124±49 3243 2770±58 1865±8
Mg 279.089 110 140 122.8±1.5 315.6±10.2 300.1±2.2 139.0±0.7
Mg 279.563 110 140 132.5±1.9 323.0±9.5 296.4±38.6 145.1±1.7
Mg 280.283 110 140 130.4±2.1 323.5±9.6 314.1±4.8 144.5±1.7
Mn 257.614 0.06 .08 0.096±0.007 1.7±0.1 1.03±0.03 N.D.
Mn 260.573 0.06 .08 0.099±0.008 1.6±0.1 1.01±0.03 N.D.
Na 330.252 560 800 730.2±14.2 477.5±6.0 676 763.7±10.3 771.1±8.6
Na 589.596 560 800 743.8±13.6 476.3±15.2 676 816.0±14.3 822.5±11.0
P 177.441 950 1050 1082±11 1404±49 1351 1547±20 1332±22
P 213.625 950 1050 1096±30 1396±38 1351 1462±27 1254±16
P 214.914 950 1050 1077±37 1382±56 1351 1432±21 1238±29
Zn 206.200 4 6.9 3.43±0.29 7.6±0.3 8.1±1.4 5.6±0.2
a Element wavelengths in Table XX also apply to Tables XXI and XXII. N.D. = None detected.

Fig. 4. Fig. 5.
Spike Spike
recover- recoveries
ies for for
milk. vanilla
bean ice
cream.

13
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ity was shown to be important to 13. CEM Application Note PM-3,
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2066-2964.
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This work also suggests that other 3. N. Miller-Ilhi, Appl. Spectrosc. 47, 14 Revision 11-91 (1991).
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15. CEM Application Note AM-5,
be analyzed effectively using ICP- 4. Instrument and Business Outlook 1, Revision 10-88 (1988).
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16. RSK-Values: The Complete Manual,
tion techniques are employed. 5. Official Methods of Analysis, 15th Verlag Flüssiges Obst, GmbH,
Ed., AOAC, Arlington, VA USA Schönborn, Germany (1987).
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17. Jus de fruits Specifications, l'Associ-
The authors gratefully acknowl- 6. The Referee 17, 9, 10-11 (1993). ation Francais de Normalisation
edge the assistance of Allan Brause, 7. L. Jorhem,. J. AOAC Int. 76, 4, 798 (AFNOR), Paris-La Defense, France
of Analytical Chemical Services of (1993). (1988).
Columbia, Inc., who provided many 8. The Referee 17, 7, 6-7 (1993). 18. J.A. McHard, S.J. Foulk, J.L.
of the authentic fruit data, to Sara 9. J.W. Jones, J. Res. Natl. Bur. Stand. Jorgensen, S. Bauer, and J.D. Wine-
Littau, of CEM Corporation for dis- (U.S.) 93, 358 (1988). fordner, in “Citrus Nutrition and
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culture Human Nutrition Informa-
tion Service Handbook Number
8–9 (revised 1982), U.S. Govern-
TABLE XXIII: ICP-OES Results for NIST SRM 1549 Milk Powder ment Printing Office, Washington,
Analyzed with Milk and with Ice Cream Samples in µg/mL DC, pp 38, 60, 90, 34, 139, 184,
269.
Element Certified SRM for Milk SRM for Ice Cream
Wavelength Value Found Found 20. United States Department of Agri-
culture Human Nutrition Informa-
Ca 315.901 13000±500 13520±128 12620±164 tion Service Handbook Number
Ca 422.671 13000±500 13360±216 13230±118 8-11(1982), U.S. Government Print-
ing Office, Washington, DC, 157.
Cu 324.767 0.7±0.1 0.8±0.5 0.54±0.03
21. United States Department of Agri-
Fe 238.207 1.78±0.1 1.86±0.15 1.82±0.06 culture Human Nutrition Informa-
Fe 239.568 1.78±0.1 2.14±0.10 1.92±0.15 tion Service Handbook Number
K 766.517 16900±300 16710±242 16500±70 8–8 (1989), US Government Print-
ing Office, Washington, DC, 107.
Mg 279.089 1200±30 1247±17 1212±2
22. L.H.J. Lajunen, J. Piispanen, and
Mg 279.563 1200±30 1264±10 1259±6 E. Saari, At. Spectrosc. 13, 4, 127
Mg 280.283 1200±30 1262±10 1236±5 (1992).
Mn 257.614 0.26±0.06 0.25±0.01 0.21±0.01 23. United States Department of Agri-
culture Human Nutrition Informa-
Mn 260.573 0.26±0.06 0.27±0.02 0.22±0.01 tion Service Handbook Number
Na 330.252 4970±100 5058±40 4813±12 8–1 (1976, revised 1990) U.S. Gov-
Na 589.596 4970±100 5136±87 5094±42 ernment Printing Office, Washing-
ton, DC, pp. 8.3, 8.4, 75, 76,
P 177.441 10600±200 10460±75 11010±258 01-077, 01-079, 01-085.
P 213.625 10600±200 10680±31 10930±73
P 214.914 10600±200 10720±52 10930±84
Zn 206.200 46.1±2.2 45.8±0.2 44.4±1.1

14