42 Poitevin: Journal of AOAC International Vol. 99, No.
1, 2016
Special GUEST EDITOR Section
Official Methods for the Determination of Minerals and Trace
Elements in Infant Formula and Milk Products: A Review
Eric Poitevin
Analytical Sciences Pillar–Minerals and Imaging Group, Nestlé Research Center, Vers-chez-les-Blanc, 1000 Lausanne 26,
Switzerland
The minerals and trace elements that account
for about 4% of total human body mass serve as
materials and regulators in numerous biological
activities in body structure building. Infant
formula and milk products are important sources
of endogenic and added minerals and trace
elements and hence, must comply with regulatory
as well as nutritional and safety requirements. In
addition, reliable analytical data are necessary to
support product content and innovation, health
claims, or declaration and specific safety issues.
Adequate analytical platforms and methods must be
implemented to demonstrate both the compliance
and safety assessment of all declared and
regulated minerals and trace elements, especially
trace-element contaminant surveillance. The first
part of this paper presents general information
on the mineral composition of infant formula and
milk products and their regulatory status. In the
second part, a survey describes the main techniques
and related current official methods determining
minerals and trace elements in infant formula and
milk products applied for by various international
organizations (AOAC INTERNATIONAL, the
International Organization for Standardization, the
International Dairy Federation, and the European
Committe for Standardization). The third part
summarizes method officialization activities by
Stakeholder Panels on Infant Formula and Adult
Nutritionals and Stakeholder Panel on Strategic Food
Analytical Methods. The final part covers a general
discussion focusing on analytical gaps and future
trends in inorganic analysis that have been applied
for in infant formula and milk-based products.
M
inerals and trace elements accounting for about 4%
of total human body mass play an important role in
bone structure, regulate certain body functions, and
in combination with water, help maintain the body’s water
balance (1). Requirements for essential nutrients, due to rapid
growth and development, specifically put infants at risk of
deficiencies of certain essential minerals (2, 3). It is therefore
Guest edited as a special report on “Modernization of Test Methods
for the Analysis of Infant Formula and Adult Nutritionals” by Darryl
Sullivan.
Corresponding author’s e-mail: eric.poitevin@rdls.nestle.com
DOI: 10.5740/jaoacint.15-0246
essential that infant formula and milk products intended for
use by infants contain minerals in amounts that satisfy their
nutritional requirements without leading to adverse effects.
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In addition, processed finished products must not contain
any toxic elements in amounts that could lead to negative
health effects (4–7). Increasingly rigorous legislation is being
enacted or discussed for regulatory compliance of declared
parameters and safety limits of toxic elements in infant formula
and milk products (8–14). Most Codex-endorsed standards
originated in the 1980s, when the Infant Formula Act was
enabled in the United States. Compliance and safety control
of new products containing, e.g., hydrolyzed protein, high
fat, and fructo-/galacto-oligosaccharides may face analytical
challenges in terms of specifity and sensitivity (15–17).
Existing standards are mostly or only partially validated
for infant formula and are generally not fit-for-purpose for
many of the new commercialized products. Moreover, the
internationally accepted analytical methods which are available
for enforcement of regulatory compliance are partly outdated,
and for some parameters are not available or nonexistent. In
particular, the range of analytical methods proposed by the
latest Codex Alimentarius for infant formula and milk products
is still inadequate, only covers a few parameters, and is in need
of major update (18).
This paper first reviews the list of minerals and ­trace-
element analytical techniques and related current official
methods from various international organizations including
AOAC INTERNATIONAL, the International Organization
for Standardization (ISO), the International Dairy Federation
(IDF), and the European Committee for Standardization (CEN)
that determine minerals and trace elements in infant formula
and milk products. This paper then covers current and future
activities in method development described in the framework
of Stakeholder Panels on Infant Formula and Adult Nutritionals
(SPIFAN) and Stakeholder Panel on Strategic Food Analytical
Methods (SPSFAM). Finally, focus on analytical gaps and
future trends in inorganic analysis applied for infant formula
and milk products for future standardization is discussed.
Minerals and Trace Elements
Definitions
Minerals are inorganic species or substances that are of neither
animal nor vegetable origin (i.e., natural compounds generally
not containing a C, H, O, or N skeleton). Inorganic elements
constitute the major part of dry ash that remains after ignition of
organic matter, and consequently dry-ashing techniques are still
the primary way to determine total minerals in foodstuffs (19).
 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016 43

Classification of minerals can be carried out according to
different methods (20) and divided, for instance, into two
groups (minerals and trace elements) as shown in Table 1 that
take into account their essentiality or well-known nutritional
concern, recommended concentration (i.e., mg/kg for minerals
or μg/kg for trace elements), and maximum limits (MLs) in
terms of toxicity.
Minerals are nutritional elements known as the main cellular
and structural building materials taking part in osmotic and acid/
base regulation [e.g., calcium (Ca), potassium (K), sodium (Na),
phosphorus (P), magnesium (Mg), and chlorine (Cl)]. Trace
elements are typically known as electrolytes, enzymes, and
hormones, constituents for which the biological roles are known
for nutritive adding value and health impact [e.g., iodine (I),

Table 1. Essentiality status, AIs, RDAs, Min and Max levels or GULs, MLs, and PTWI for minerals and trace elements in
infant formulaa

AI or RDA*, mg/d from www.nap.edub Min–Maxc levels/ GUL,d

e
Essentiality status for infants mg/100 kcal; or ML, μg/kg;
f
Element category Elements (symbol) from WHO guideline (4) Infants 0–6 mo Infants 7–12 mo or PTWI, μg/kg bw

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Minerals Calcium (Ca) Essential 210 260 50c–140d,g
Magnesium (Mg) Essential 30 75 5c–15d
Sodium (Na) Essential 120 370 20c–60c
Potassium (K) Essential 400 700 60c–180c
Phosphorus (P) Essential 100 275 25c–100d,g
Chlorine (Cl) Essential 180 570 50c–160c
Trace elements Iron (Fe) Essential 0.27 11* 0.45c–ND
c d
Zinc (Zn) Essential 2 3* 0.5 –1.5
Copper (Cu) Essential 0.20 0.22 0.035c–0.12d
Chromium (Cr) Essential 0.0002 0.0055 1.5c–10d
Molybdenum (Mo) Essential 0.002 0.003 1.5c–10d
Selenium (Se) Essential 0.015 0.020 0.001c–0.009c
Iodine (I) Essential 0.11 0.13 0.01c–0.06d
Cobalt (Co) Essential ND ND ND
Manganese (Mn) Essential/potentially toxic 0.003 0.6 ND
e,h
Fluorine (F) Essential/potentially toxic 0.01 0.5 0.100
Boron (B) Probably essential ND ND ND
Silicon (Si) Probably essential ND ND ND
Nickel (Ni) Probably essential ND ND ND
Vanadium (V) Probably essential ND ND ND
Lithium (Li) Probably essential ND ND ND
e,i
Tin (Sn) Potentially essential/toxic ND ND 50c000
Arsenic (As) Toxic/potentially essential ND ND 15d
Cadmium (Cd) Toxic/potentially essential ND ND 7d
e,j
Lead (Pb) Toxic/potentially essential ND ND 20 (25f)
f
Mercury (Hg) Toxic/potentially essential ND ND 5
Aluminum (Al) Toxic/potentially essential ND ND 1000f
Bromine (Br) Toxic/potentially essential ND ND ND
a
 AI = adequate intake; bw = body weight; GUL = guidance upper level; Max =maximum; Min = minimum; ML =; maximum limit; ND = not determined;
PTWI = provisional tolerable weekly intake; RDA = recommended dietary allowance; WHO = World Health Organization; * = RDA intake values (only
for Fe and Zn elements).
b
 AI and RDA values taken from dietary reference intake (DRI) reports, Food and Nutrition Board, Institute of Medicine, National Academies (see www.
nap.edu).
c
 Min and Max levels in ordinary style from Codex Standard (8).
d
 GULs in boldface set instead of Max level from Codex Standard (8).
e
 Codex MLs in italic style from Codex Standard (21).
f
PTWIs in italic and boldface from Codex Standard (21).
g
The Ca:P ratio shall be <1.0 and not >2.0.
h
Codex MLs for F set at ML = 100 μg per 100 kcal in ready-to-feed infant formula.
i
 Codex an EC MLs for inorganic Sn set at ML = 50 mg/kg fresh weight and the same level for preparations for infant formulae and follow-on formulae
and for canned dietary foods for special medical purposes specifically for infants (not including dried and powdered products).
j
Codex MLs for Pb set at ML = 0.020 mg/kg fresh weight.
44 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016
iron (Fe), copper (Cu), chromium (Cr), molybdenum (Mo),
selenium (Se), manganese (Mn), zinc (Zn), and cobalt (Co)].
Some trace elements still have unknown or limited/restricted
beneficial impact on metabolic and physiological functions
[e.g., fluorine (F), boron (B), silico (Si), nickel (Ni), vanadium
(V), lithium (Li), and antimony (Sb)] (20). Some other elements
are either regulated additives: aluminum (Al), sulfur (S) as
sulfites and sulfates, bromine (Br) as bromides and bromate salts
or strictly controlled toxic contaminants with known negative
health effects, such as arsenic (As), cadmium (Cd), lead (Pb),
mercury (Hg), and tin (Sn; 21, 22). Moreover, several minerals
and trace elements can also be part of adulterant compounds
intentionally added to foodstuffs for economic and/or criminal
reasons (e.g., authenticity and/or fraud and tampering) and
which lessen the purity or effectiveness of foodstuffs, causing
an undesirable effect with safety risks and damaged integrity by
possible loss of beneficial substance properties (23, 24).
Inorganic Composition of Infant Formula and
Milk Products
Minerals (e.g., Ca, P, K, S, Na, Mg, and Cl) and some trace
elements (Fe, Zn, Mn, Cu, and I) account for 3.5 and 0.5%,
respectively of total human body mass (1). Ca, P, and Mg are
mainly distributed in bones and skeletal tissues ranging from
70 to 80% for Mg and P to 99% for Ca. Iodine is largely stored
in thyroid tissue, Co is part of vitamin B12, and other trace
elements (Fe, Zn, Mn, Cu, and I) are partly stored in every
tissue, liquid, cell, and organ in the human body as part of a
protein, enzyme, and hormone. Mineral content constitutes
a small part of raw milk (i.e., 7–9 g/L), mainly including Ca,
K, Mg, Na, Cl (as chloride), and P (as phosphate). Ca and P
especially play important roles in the structure and stability of
the casein micelles. Most Cu, Zn, and Mn is bound to casein
whereas Fe partly binds to lactoferrin. Iodine is assumed to be
in its iodide form and mainly found in whey fraction, and Se is
mainly linked to protein fraction (1, 25). The levels at which
minerals are present in infant formula and milk products are the
result of a dynamic equilibrium of minerals between aqueous
Table 2. International and specific national regulations for infant nutritiona
Legislation Infant formula
a
Codex Alimentarius Commission FAO/WHO (2007)
(International)
Codex Standard 72- 1981
Revised Section A
United States a
FDA (1985, 2007a,b)
Infant Formula Act
a
21 CFR 107
European Union (EU) EU (2006b) Commission
a
Directive 2006/141/EC
Australia and New Zealand Food Standards Australia and New
Zealand Standard 2.9.1a
China GB 10765- 2010 (infant formula and
follow- on formula)
a
CFR = Code of Federal Regulations; EC = European Community; FAO = Food and Agricultural Organization; FDA = U.S. Food and Drug ­Administration;
b
NA = Not applicable.
and colloidal milk phases, technological treatment (e.g., reverse
osmosis, membrane ultrafiltration, fortification, and spraying),
and mineral fortification applied during the manufacturing
process. The mineral composition of infant formula and milk
products is the result of several factors, including process,
nutritional, and regulatory requirements (15, 25).
Regulations and Limits
The primary objective of regulatory bodies is the protection
of consumers and especially the regulation of infant nutrition.
Primary legislation on compliance (i.e., mineral composition and
nutrient requirements for infant formula) is displayed in Table 1
and presented in terms of adequate daily intake, recommended
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dietary allowances, minimum/maximum levels, or guidance
upper level. Safety control of toxic elements for infant formula
and milk products is also shown in Table 1 in terms of MLs
and provisional tolerable weekly intake. Regulations for
infant formula and milk products are detailed in international
standards elaborated either by Codex Alimentarius Commission
under the authority of Food and Agricultural Organization of the
United Nations and the World Health Organization or in specific
standards elaborated by mainly European Union, United States,
China, Australia, and New Zealand as displayed in Table 2
(8–14, 21, 22). Besides strictly regulated food additives that
are intentionally added to provide specific and well-defined
actions in the final product, inorganic contamination from raw
materials, the process, or intentional adulteration/fraud for
authentication are also regulated by standards elaborated by the
above-mentioned national or international organizations and
authorities.
Determination of Minerals and Trace Elements
Mineral analysis in food samples generally requires a
preliminary step of sample preparation, including a dissolution
or homogenization step (e.g., blending, mixing, grinding, or
slurry preparation) of the laboratory sample, then a collection
of a representative test portion, and finally decomposition
Follow-on formula Formula for special medical purpose
FAO/WHO (1987) Codex FAO/WHO (2007)
­Standard 156
Codex Standard 72-1981
Revised Section B
NAb FDA (1985, 2007a,b)
Infant Formula Act
21 CFR 107
EU (2013) EU (2013)
Council directive 609/2013 /EC Council Directive 609/2013/EC
 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016 45
through acid- or alkaline-assisted hot digestion with or
without high pressure. The digestion step involves the acid
dissolution of dry ash, wet acid, or alkaline digestion/extraction
by conventional conductive or microwave heating in a
combination of concentrated acids or extraction of elements
and inorganic species with an organic, alkaline, or acid buffer.
The final sample digest is commonly diluted in an acidic or
alkaline aqueous solution and, as a result, easily amenable to
any analytical technique (26).
History
Thirty years ago potentiometry using ion-selective electrodes
(ISEs), titrimetry, spectrophotometry, and anodic stripping
voltammetry (ASV) were historically and traditionally
techniques of choice for mineral determination in infant
formula and milk products; they generally only needed a matrix
dissolution with water or buffer and did not require preliminary
matrix decomposition using digestion techniques (26). Oldest
official methods are mainly based on these techniques but they
suffer of specific analytical interferences and of their limitations
to single-analyte determination. Development of decomposition
techniques like open dry ashing with muffle furnace at 450–550°C
and further open wet-ashing techniques had significantly
enlarged the inorganic analytical field to atomic absorption
spectrometry (AAS) and atomic emission spectrometry (AES).
The closed wet-digestion technique using high-pressure
digesters [e.g., microwave or high-pressure ashing (HPA)
systems with a combination of acids, such as nitric acid (HNO3)
and hydrochloric acid (HCl)] allows significant reduction
of the residual carbon content (RCC) of digest samples with
an RCC <30 mg/g. Nowadays, the most commonly used
digestion technique for minerals and trace elements is high-
pressure digestion using a closed-vessel microwave system.
It allows high-sample throughput, significantly minimizes
losses during oxidation, avoids any reaction between minerals
and vessels, and reduces contamination risk (mainly for trace
elements) before analytical measurement. Classical dry-ashing
digestion is mostly used and recommended for total ashing
determination (19).
AES technique using either a classical flame source [flame
emission spectroscopy (FES)] or plasma source [inductively
coupled plasma-atomic emission spectrometry (ICP-AES)]
is the oldest and most widely used multianalyte technique for
mineral nutrient analysis. In the 1980s, AAS was first used
with a flame atomization source (FAAS) and later a graphite
atomizer [graphite furnace (GF)AAS] was increasingly adopted
as the reference spectrometric technique for trace element
analysis. Use of other furnace atomizers and releasing or
protective agents [e.g., lanthanum (La), strontium chloride,
EDTA and Zeeman effect background-correction techniques
use electrothermal AAS technique as the preferred method for
trace element analysis because of its increased sensitivity and
spectral interference removal ability (26, 27).
Among other atomization techniques for AAS and AES,
hydride generation AAS (HGAAS) and AES are commonly
used for unstable elements like As, Se, and Sb. Cold vapor AAS
(CVAAS) is specifically used for Hg determination at low levels
of concentration in food matrixes (26–28). Coupling an ICP
source with a mass spectrometer (ICP-MS) after high-pressure
digestion is currently the best technology for mineral analysis
in food digest samples (26). Quadrupole mass spectrometers
are the most commonly used commercial equipment in ICP-MS
technology (i.e., approximately 85% of all ICP-MS instruments
used today) for routine analysis with low resolution (i.e., only
at unit mass). ICP-MS technology is definitely the multianalyte
technique of choice to obtain equivalent or better instrumental
detection limits in solution (i.e., ng/L) than those from FAAS,
ICP-AES or GFAAS, HGAAS, and CVAAS (26, 29–31).
Moreover, ICP-MS detectors allow samples with varying
analyte concentrations to be analyzed together because of their
wide analytical working range (i.e., 9 orders of magnitude). The
combination of wide analytical working range and excellent
sensitivity allows for short ICP-MS analysis times, reduced
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sample-handling requirements, minimized potential analytical
errors, and avoiding the need to frequently recalibrate the
system as compared with other atomic spectrometry techniques
(29–31). Major limitations of ICP-MS equipment are high
initial investment; a need for qualified operators; and the high
cost of consumable supplies, gas [i.e., argon (Ar)], and high
power requirements compared with other atomic spectroscopic
techniques (30).
Alternative nondestructive techniques like X-ray fluorescence
(XRF) after calibration with another atomic spectrometry
technique or costly and complex neutron activation analyzer
are also still but less extensively used in routine food control
(26, 28).
Review of Current Official Methods
Various international organizations including AOAC
INTERNATIONAL, ISO, CEN, the European Nordic
Committee (NMKL), and IDF have published official methods
of analysis for several parameters declared in infant formula
and milk products (32–34). Many of these methods displayed in
Tables 3 and 4 are Codex-adopted methods for foods including
infant formula and milk products but are 20–30 years old, and
only a few have been updated (18). Other national standards
validated for infant formula and milk products but not listed
in the tables are also available from China [Guobiao (GB)]
and Australia and New Zealand [Australian Standards (AS)].
The principles of the most currently used multianalyte official
methods are based on a preparation of a representative test
sample (AOAC 985.30, European norm EN 13804:2013), then a
mineralization step in the test portion that is generally performed
by dry-ashing or high-pressure digestion. High-pressure
digestion involves the use of either open- or closed-vessel
microwave digestion with a combination of HNO3 and HCl
and occasionally hydrogen peroxide (H2O2) or HPA with HNO3
only (EN 13805:2013). After appropriate dilution, digested test
solutions are generally analyzed with an atomic spectrometric
technique (FES, FAAS, GFAAS, ICP-AES, HGAAS, or
ICP-MS) standardized with acid (or alkaline buffer for I and
Br)-matched standard calibrant solutions. Some older official
methods use other analytical techniques without a digestion
step (e.g., spectrophotometry, HPLC, potentiometry, titrimetry,
fluorometry, and ASV) but their scope is generally limited to
the single-analyte determination of free element forms (e.g.,
Ca, P, Cl, F, Fe, Cu, Se, Sn, As, and Hg).
46 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016

Minerals.—Analysis of nine minerals (Ca, Mg, Na, K, P, Fe,
Zn, Cu, and Mn) in infant formula and milk products are more
or less covered by FAAS (e.g., AOAC 985.35, ISO 8070/IDF
119:27, AOAC 999.11/NMKL 161:1998, and AOAC 999.11/
NMKL 139:1991) or ICP-AES (AOAC 984.27, AOAC 2011.14,
and ISO/CD 15151/IDF 229) procedures after dry ashing or high-
pressure digestions. AOAC 2011.14 is a modernized version of
AOAC 984.27 with improvements involving the use of optimized
microwave digestion, axial and radial ICP-AES configurations,
selected analytical lines, internal standardization, ion buffering for
an enlarged scope, and fortified food products covering the AOAC
food triangle including infant formula and milk products (35, 36).
Several Codex type II, III or IV methods are applied in
infant formula and milk products for P (AOAC 986.24), Fe
for Zn by AAS (AOAC 969.32); and for Ca using titration (ISO
12081/IDF 36:2010).
Chlorine is generally analyzed in its inorganic chloride form
−
(Cl ) in infant formula (AOAC 986.26) or in special foods
(AOAC 971.27) by potentiometry.
Trace Elements.—Trace elements (Cr, Mo, Se, As, Cd, Hg, Pb,
and Sn) are mainly determined by sensitive atomic spectrometric
techniques (i.e., GFAAS, HGAAS, ICP-MS) after either dry
ashing or high-pressure digestion using generally closed vessels.
Inorganic iodide (I−) has been historically and still is currently
determined in infant formula by either potentiometry (AOAC
992.24) using ISE or by HPLC-EC (AOAC 999.22, ISO
14378:2009/IDF 167). Today the ICP-MS technique is used to
determine total iodine (i.e., sum of added iodide and endogenous

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(ISO 6732/IDF 103:2010), and Cu (ISO 5738/IDF 76) by iodine forms) through the recently issued AOAC Method
spectrophotometry; for Na and K using FES (AOAC 990.23); 2012.14 or AOAC Method 2012.15 (37, 38). Another official

Table 3. Official multianalyte methods for infant formula (IF) and milk productsa

Codex type (I, II, III) or

Analytes Official method/project No. Technique Scope official status
All AOAC 985.30 Sampling and mixing IF Final Action 1988
All EN 13804:2013 Sampling Foods Revised 2013
All (ash) AOAC 942.05 Gravimetry Foods I
All EN13805:2013 High-pressure digestion Foods Revised 2013
Ca, Mg, Na, K, P, Fe, Mn, Cu, AOAC 984.27 ICP-AES IF III
Zn, (S)
AOAC 2011.14 ICP-AES Foods fortified products Final Action 2013
ISO/CD 15151, IDF 229 ICP-AES Milk products Adopted 2010
Ca, Mg, Na, K, Fe, Mn, Cu, Zn AOAC 985.35 FAAS Foods, IF II
Ca, Mg, Na, K ISO 8070:2007, IDF 119:2007 FAAS IF, milk products II
Fe, Cu, Zn, Cr, Pb, Cd EN 14082:2003 FAAS Foods, IF (Cr) II (for Cr – Section B of
b
STAN72 only)
GFAAS Adopted 2003
EN 14084:2003 FAAS Foods Adopted 2003
Mo, Cr, Pb, Cd EN 14083:2003 GFAAS Foods, IF (Cr) III (for Cr – Section B of
STAN 72 only)
Fe, Cu, Zn, Pb, Cd AOAC 999.10, NMKL 161:1998 FAAS Foods, IF (Fe) First Action 1999
GFAAS Revised 2002
AOAC 999.11, NMKL 139:1991 FAAS Foods II
GFAAS
As, Se, Zn, Pb, Cd AOAC 986.15 HGAAS Foods Final Action 1988
ASV Revised 1996
III (Cd, Pb, Zn)
As, Cd, Hg Pb AOAC 2013.06 ICP-MS Foods First Action 2013
EN 15763:2009 ICP-MS Foods Adopted 2009
Cr, Mo, Se AOAC 2011.19 ICP-MS IF First Action 2011
Na, Mg, Ca EN 15505:2008 FAAS Foods Adopted 2008
Na, K AOAC 990.23 FES Foods First Action 1990
As, Se EN 14627:2005 HGAAS Foods III (Se)
Mo, Se AOAC 2006.03 ICP-AES IF III (For Mo–Section B of
STAN 72 only)
Pb, Cd AOAC 992.23 ASV Foods III (Pb)
a
IF = Infant formula.
b
STAN72 = Standard for Infant Formula (CODEX STAN 72-1981)
 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016 47

Table 4. Official single-analyte methods for infant formula (IF) and milk products

Codex Type (I, II, III) or

Analytes Official method/project No. Technique Scope official status
Ca ISO 12081:2010, IDF 36:2010 Titrimetry Milk Adopted 2010
P AOAC 986.24 Spectrophotometry IF II
AOAC 995.11 Spectrophotometry Foods, IF First Action 1995
ISO 9874, IDF 42:2006 Spectrophotometry Milk Adopted in 2006
Fe ISO 6732:2010, IDF 103:2010 Spectrophotometry Milk products IV
Cu ISO 5738, IDF 76:2004 Spectrophotometry Milk products III (whey powder)
AOAC 960.40 Colorimetry Foods III
Zn ISO 11813:2010, IDF 156:2010 FAAS Milk products Revised 2010
AOAC 969.32 AAS Foods III

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Iodine as iodide or total iodine AOAC 2012.14 ICP-MS IF First Action 2012
AOAC 2012.15 ICP-MS IF First Action 2012
EN 15111:2008 ICP-MS Foods Adopted 2008
AOAC 992.24 Potentiometry IF II
AOAC 925.56 Titrimetry Foods II
AOAC 992.22 HPLC Milk products First Action 1992
ISO 14378:2009, IDF 167 HPLC Milk products Adopted 2009
Fluorine as soluble fluoride LMBG-L 49.00-7 Potentiometry IF Adopted 2000
AOAC 961.16 Titrimetry Foods Final Action
Chlorine as chloride AOAC 986.26 Potentiometry Foods, IF III
Se AOAC 996.16 HGAAS IF III
AOAC 996.17 HGAAS IF III
AOAC 974.15 Fluorimetry Milk powder Final Action 1976
Revised 1996
As EN 14546:2005 HGAAS Foods Adopted 2005
Hg AOAC 971.21 Flameless AAS Foods Final Action 1976
AOAC 952.14 Colorimetry Foods Final Action 1952
EN 13806:2002 CVAAS Foods Adopted 2002
Pb AOAC 972.25 AAS Foods whey powder III
II (whey powder)
a b
ISO/TS 6733:2006, IDF/RM GFAAS Milk products Adopted 2006
133: 2006
AOAC 982.23 ASV Foods III
Sn AOAC 985.16 FAAS Canned foods Final Action 1988
EN 15764:2009 GFAAS/FAAS Foods Adopted 2009
EN 15765:2009 ICP-MS Foods Adopted 2009
ISO 14377:2002, IDF 168:2002 GFAAS Canned evaporated milk Adopted 2002
ISO/TS 9941:2005, IDF/RM Spectrophotometry Milk and canned Adopted 2005
160:2005 ­evaporated milk
a
TS = Technical Specifications;
b
RM = Reviewed Method.

method using ICP-MS (EN 15111:2008) has procedure in
principle similar to the previously cited AOAC Methods but had
not been initially validated for infant formula and milk products.
No international official methods exist for fluorine (F)
determined as its soluble fluoride part in infant formula.
A German method (German Food Law standard 49.00-17) using
ISE is available and has been validated for dietetic products.
However, low levels of F are rather difficult to analyze with this
technique in recent infant formula used for medical purpose.
Determination of Cr, Mo, and Se are also somewhat
problematic using GFAAS and HGAAS due to their typical
presence in trace levels in infant formula and healthcare
products. However a recent official method using ICP-MS after
microwave digestion (AOAC 2011.19) is now available for
the simultaneous determination of the three analytes in infant
formula and adult nutritionals (39). Other official methods exist
for Se determination by HGAAS specifically in infant formula
(AOAC 996.16 and AOAC 996.17) as well as in foodstuffs (EN
48 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016
14627:2005, AOAC 986.15). Cr in infant formula and Mo in
foodstuffs can also be determined by GFAAS after dry-ashing
(EN 14082:2003) or pressure digestion (EN 14083:2003). Most
cited official methods have a Codex type II or III status but have
been partly validated for infant formulas and/or milk products.
Some methods are well-regarded but not Codex-approved,
except for Section B of Codex Standard 72 (8).
Many official methods exist for determination of regulated
toxic trace elements, mainly including heavy metals (As, Cd,
Hg, Pb, and Sn) generally in foods but partly in infant formula
and milk products. Methods using either AAS after dry-ashing
(AOAC 999.11/NMKL 139:1991) or microwave digestion
(AOAC 991.10/NMKL 161:1998) are used for Pb and Cd in
all foods. Another Codex type III method (AOAC 986.15) uses
ASV to determine both heavy metals. Other official methods
are available for Cd and Pb determination by FAAS after dry-
ashing (14082:2003) and by FAAS/GFAAS after high-pressure
digestion (EN 14083:2003, EN 14084:2003) in foodstuffs. ICP-
MS methods after high-pressure digestion (EN 15763:2009,
AOAC 2013.06) are good multianalyte method candidates
but do not specifically cover infant formula and milk product
categories. Codex type III methods exist for Pb determination
in milk and milk products by GFAAS (ISO/Technical
Specifications 6733:2006) and by FAAS (AOAC 972.25).
Official methods are available using HGAAS after
dry-ashing or pressure digestion for total As in foodstuffs
(AOAC 986.15, EN 14546:2005, EN 14627:2005, EN
14332:2004). Total Hg can be determined by CVAAS (EN
13806:2002), FAAS (AOAC 971.21, AOAC 977.15, AOAC
974.14), colorimetry (AOAC 952.14), or ICP-MS after high-
pressure digestion (EN 15763:2009, AOAC 2013.06).
Finally, Sn that is specifically regulated in canned foods is
currently determined by GF–AAS/F–AAS (AOAC 986.15,
EN 15764:2009, ISO/TS 9941:2005/IDF/Reviewed Method
160:2005) or more recently by ICP-MS after pressure digestion
(EN 15765:2009) even if they are not Codex type methods
specifically for infant formula.
Past, Current, and Future SPIFAN and SPSFAM
Activities
AOAC INTERNATIONAL reached an agreement on 2010
with the International Formula Council (IFC) on a 2-year
project to form SPIFAN and to create Standard Method
Performance Requirements (SMPRs®), published as standards
for methods focused on nutrients in infant formula and adult
nutritionals. The SPIFAN project was supported by the infant
formula industry to establish and use recognized international
reference standards for key nutrients found in infant and adult
nutritionals. This first SPIFAN initiative (SPIFAN I) included a
list of priority (pseudo) vitamins, nucleotides, trace mineral I,
and ultra-trace elements (UTEs) Cr, Mo, and Se.
SMPRs were hence established and published as a consensus
standard developed by stakeholders in a very controlled
process that ensures users, research organizations, government
departments, and consumers work together to create a standard
that meets the demands of the analytical community and
technology (40). SMPRs prescribe the minimum analytical
performance requirements for classes of analytical methods
in terms of analytical range, specificity, limits of detection and
of quantitation, repeatability, recovery, and reproducibility. A
kit of 12 representative infant formula and adult nutritionals
matrixes, including National Institute of Standards and
Technology (Gaithersburg, MD) Standard Reference Material
1849 (41), was provided by manufacturers for single-
laboratory validation (42, 43) of selected methods by an AOAC
INTERNATIONAL expert review panel (ERP). The SPIFAN I
process for minerals has resulted in two published SMPRs for
simultaneous determination of UTEs Cr, Mo, and Se (SMPR
2011.009) and total iodine (SMPR 2012.008). Then two AOAC
Methods for iodine (AOAC 2012.14 and AOAC 2012.15) and
one for Cr, Mo, and Se (AOAC 2011.19) received First Action
Official Method status by the Official Method Board (OMB).
AOAC Method 2011.19 for UTEs (Cr, Mo, and Se) and AOAC
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Method 2012.15 for iodine were finally recommended by the
ERP to undergo multilaboratory testing for the Final Action
step. The OMB approved AOAC Method 2011.19 for Final
Action status on November 2014 as recommended by the
AOAC ERP.
In parallel, SPIFAN II was signed in mid-June 2013 to
continue to focus on completing the nutrient panel through
September 2016. In August 2013, AOAC launched nine
minerals: Ca, Mg, Na, K, P, Fe, Mn, Cu, and Zn. The next set
of nutrients for mineral analysis to be launched was fluoride
and chloride in March 2014. The SMPRs for minerals were
developed by the Minerals Working Group, approved by
stakeholders, and then published in 2013 (SMPR 2014.004).
Finally, SMPRs for chloride and fluoride were afterwards also
approved on September 2014.
In parallel a SMPR has been completed for As, Cd, Hg, and
Pb in a variety of foods, including infant formula by the Heavy
Metals Working Group, and was endorsed in 2012 as AOAC
SMPR 2012.007 by SPSFAM. A fitness-for-purpose statement
for heavy metals speciation in foods (and beverages) was
endorsed by SPSFAM in 2014. At the end of 2014, the Heavy
Metals Speciation Working Group developed a draft SMPR
dedicated to heavy metals speciation for the determination
of the major toxic chemical species present in selected food
and beverage matrixes for any of the following elements: As
(priority target), Hg, and Cr.
Moreover, a cooperation agreement was signed in 2012
between ISO and AOAC INTERNATIONAL. This new
partnership allows for the joint development and approval of
common standards focusing in priority areas through SPIFAN
activities in milk and milk products, infant formula, and adult
nutritionals.
This existing agreement between ISO and AOAC
INTERNATIONAL also involves collaboration with IDF
relating to their joint program of work on methods of analysis
and sampling of milk and milk products. This ISO-AOAC
agreement and IDF collaboration broadens global acceptance of
standards to facilitate international trade of infant formula, adult
nutritionals, and milk products for the benefit of all stakeholders
and consumers.
Finally, the AOAC China Section and AOAC SPIFAN with
the involvement of Chinese authorities successfully held a
2014 symposium on new analytical challenges and solutions in
China. This allows resolution of new analytical challenges and
the comparison of AOAC and Chinese standard methods (GB)
in food analysis, especially infant formula and milk products.
 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016 49
Moreover, during this symposium, experts from international
organizations, governments, competent authorities, universities,
relevant testing agencies, instrument companies, and dairy
manufacturers helped bridge the gap between AOAC and GB
methods, by aligning the related standards, which will promote
method development, as well as benefits consumers worldwide.
Analytical Gaps and Trends in Inorganic Analysis
As discussed, determination of whole essential and
nonessential/toxic elements in foods today are covered by many
analytical standards, but a great part of these official methods
are either antiquated or do not provide multianalyte features
and therefore unfit for purpose determination in a defined scope.
Analytical gaps must be filled mostly to answer fitness-for-
purpose for increasingly strict regulations and safety controls of
mineral nutrients and certain element species in matrixes with
complex compositions in current and future infant formula,
adult nutritionals, and milk products.
Sample pretreatment is still the most time-consuming step
in routine analytical procedures and hence the bottleneck in
the entire analytical process, when minerals or trace elements
have been determined in solid food matrixes. Advancements
in wet-acid digestion using popular high-pressure microwave
-assisted procedures must continue along with the development
of safer and simpler systems and a significant time-reduced
digestion program to allow high-sample throughput and better
efficiency resulting in low RCC in digest samples (44-46).
Development and further officialization of multianalyte
methods simultaneously analyzing minerals and trace elements
must be favored using, e.g., emerging ICP-MS equipped with
new collision and reaction cell (CRC) technologies and inert/
reactive gas (e.g., helium, hydrogen, ammonia, methane,
oxygen) to minimize isobaric and polyatomic interferences
(47–55).
If the determination of nine minerals, chloride and fluoride
in infant formula will be soon covered by SPIFAN II process
and their related recently approved SMPRs, other more or less
regulated, specifically added or occurring contaminant elements
during food processing like Co, B, Al, Ni, Sb, Si, titanium (Ti),
and V are partly or still not determined by current international
standards.
Some international standards exist to analyze certain element
species in foods (e.g., inorganic arsenic, methylmercury, methyl
bromide, and organotins) but lack specifically in infant formula
and milk products. Beyond As and Hg speciation concern, other
anionic species of N, P, and S are either used as additives in
their oxide anionic forms (e.g., nitrite, nitrate, sulfites, sulfates,
and phosphates) or process contaminants that need to be better
controlled with further renovation or adaptation of existing
standards (e.g., ion chromatography) to include the scope of
infant formula and milk products.
Aside from the development of robust, rapid, sensitive, accurate,
and sustainable instrumentation and methodologies that provide
multianalyte capabilities with high-sample throughput (e.g.,
microwave -assisted digestion, ICP-MS), it turns out that green
analytical chemistry (GAC) is recognized as a stimulant to reduce
the negative impact of chemical analyses on the environment and
facilitates or enables implementation of sustainable development
principles in analytical laboratories (56).
Today automation, miniaturization, reduction of energy,
and multianalyte determination in a single analytical cycle
and wider use of hyphenated techniques are considered the
main way to green analytical laboratories (57). Ideally, a
green method in atomic spectrometry should avoid the use of
toxic/hazardous reagents and involve small reagent/sample
consumption, energy-efficient apparatus, safe operations,
and short total times for analysis (58). Most current official
analytical methods cannot be considered green and therefore
need specific improvements. In this context, GAC cannot be
ignored as a significant concept for methods of choice before
being proposed for any standardization.
In this GAC context, an example of such a new approach is
called single-reaction chamber (SRC) technology, which was
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launched to potentially overcome the limitations of traditional
microwave sample preparation. The heart of the system is a
sample chamber that is pre-pressurized with inert gas and heated
with microwave energy and serves both as a microwave cavity
and reaction vessel. It allows the implementation of efficient and
rapid digestions of mixed batch of samples using concentrated
or diluted solutions of HNO3 with extremely simple heating
programs at high pressures and temperature. The feasibility
of this technology was demonstrated for certified reference
materials including whole milk powder (59). If slurry-sampling
techniques before atomic spectrometry are also continuously
developed mainly for micro- or liquid samples, sample
preparation in speciation is today focused on microextraction
procedures, solid-phase extraction, and ultrasound-assisted
extraction (UAE; 60). UAE techniques using either ultrasonic
baths or probes with or without the use of enzyme have to be
considered in the near future; extraction techniques are mainly
efficient for speciation, significantly reducing working times,
minimizing interconversion of species forms, and increasing
both the yields and quality of extract (61).
Newly commercialized equipment using microwave-induced
plasma–atomic emission spectrometry (MIP-AES) have been
launched with claims of wider linear dynamic range and
greater detection limits and analysis speed compared with
conventional FAAS apparatus (62). Based on atomic emission
technique, this elemental analysis technique, equipped with a
novel magnetically excited plasma coupled to a fast sequential
monochromater, produces simpler spectra than ICP-AES and
is more sensitive than FAAS. Unlike ICP technology which
generally uses radio frequency-induced plasma, MIP-AES
uses an electrical field coupled with microwave energy to
generate robust and stable plasma using air or nitrogen gas. The
nitrogen-based plasma operates from a compressed air supply
and nitrogen generator, resulting in significant cost reductions
in operation and infrastructure by eliminating the flammable
and/or expensive gas requirements and costly consumables
typically used in FAAS (e.g., hollow cathode lamps) and
ICP-AES techniques (e.g., argon).
Moreover, the first commercialized triple quadrupole
ICP-MS/MS instrument, equipped with an octopole collision
cell located between two quadrupole mass filters, provides the
first promising results on quantification of S and P elements
in proteomics (63). This approach could provide an elegant
approach via a precursor ion and/or product ion scanning to
solve even the most challenging cases of spectral overlap and
interference (e.g., Cr, As, Se, P, S, Si, Ti, and Fe). This equipment
50 Poitevin: Journal of AOAC International Vol. 99, No. 1, 2016
will be the first with the ability to provide a true multianalyte
method for simultaneous analysis of minerals and trace elements
in food matrixes. Conceivably, this new and powerful approach
will also boost ICP-MS quantitative applications in fields such
as nanotechnology for the characterization and further control
of engineered inorganic nanoparticles in processed foods.
High resolution mass spectrometers combining magnetic
and electric sector field analyzers are also occasionally used
to overcome limitations from the polyatomic ion spectral
interferences (29). However, routine analysis using such costly
equipment necessitates even more skilled operators and regular
maintenance.
Speciation analysis of toxic elements (e.g., As, Hg) in specific
foods (e.g., seafood, rice, etc.) by coupling LC or SPE to atomic
spectrometry techniques (AAS, ICP-MS) is increasingly
covered by current or draft official methods, but the challenge
remains determining element species at low concentrations in
food due to the complex chemical behavior and instability of
species during extraction and/or the analytical step. However,
LC-ICP-MS and other hyphenation with GC will undoubtedly
play a crucial role in the next decade in establishing updated
standards for currently regulated As, Hg and Sn. More recently,
field-flow fractionation coupled with ICP-MS seems to be a
promising hyphenated technique for the determination of Ag,
Si, and Ti inorganic nanoparticles in processed foods (64–66)
in the frame of authenticity and potential adulteration of infant
formula and milk products. Official speciation methods will
also be developed in the near future for some essential elements
(e.g., I, Se, Fe, Zn, and Co) for nutritional health and claims.
For example, determination of vitamin B12 in infant formula
and milk products has historically been carried out routinely
with official methods using microbiological assay (MBA),
which is time-consuming and labor-intensive. LC emerged as
an efficient technique to determine vitamin B12 and three LC
official methods were issued (AOAC 2011.08, AOAC 2011.09,
and AOAC 2011.10). However, traditional LC methods (i.e.,
without tandem mass spectrometry detectors) lack sensitivity,
and most procedures require cleanup and preconcentration
steps to increase the ability to measure low concentrations of
vitamin B12. Hence, a recent paper shows that the combination
of LC-ICP-MS using collision cell technology and reversed-
phase LC could provide promising feasibility to separate and
selectively detect different cobalamin forms (e.g., hydroxo-,
cyano-, adenosyl-, and methyl-cobalamins), minimizing matrix
interference accomplished through the measurement of the Co
content of LC peaks (67, 68).
Finally, different solid-sampling techniques must be
continuously explored for their potential feasibility to analyze
elemental information in solid samples without matrix
pretreatment, dissolution, or digestion. The main techniques for
elemental analysis in foodstuffs and especially in milk-based
powders that could be explored in the next decade are XRF
(69, 70), solid sampling coupled with GFAAS (SS-GFAAS),
solid-sampling electrothermal vaporization coupled with
ICP-MS (SS-ETV-ICP-MS), laser ablation coupled with
ICP-MS (LA-ICP-MS), and glow discharge coupled with MS
(56, 57, 71).
Conclusions
Most of the official methods currently used and validated
for the determination of minerals and trace elements in infant
formula and milk products are multielemental based on AAS
and ICP-AES techniques after dry-ashing or high-pressure
digestion. A review of the various official methods of analysis
for infant formula from AOAC, ISO, EN, and IDF shows that
considerable gaps are present in the portfolio of official methods
available. Moreover, many of these methods and additional
single-analyte methods are outdated and in some cases poorly
validated for the scope.
Reinforced AOAC/ISO-IDF collaboration and recently
approved or issued SMPRs and AOAC methods by SPIFAN
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and SPSFAM will allow the establishment of reliable dispute-
resolution methods for the analysis of minerals and trace
elements in infant formula and milk products. Heavy metals and
inorganic additives will also be progressively included, even if
official updated multielemental methods lack some elements
(e.g., Al, Co, V, B, Ni, Sb, and Br) and oxide anions (e.g., nitrite,
nitrate, phosphate, and sulfite) contain N, P, and S, and generally
are found as counter anions of food additives and grade salts.
ICP-MS following microwave-assisted acid digestion is
undoubtedly the fastest and most unique growing trace element
technique commercially available today in combination with
well-established integrated revolutionary CRC technology.
The main reason for its success is this technique’s ability to
carry out rapid multielement determination at trace levels with
limited interferences. This technique has been recently gaining
in popularity because it is becoming less complicated, less
expensive, and no longer requires highly skilled staff to carry
it out.
Future methods for standardization will progressively
integrate the green inorganic analysis trends such as
sustainability, simplicity, miniaturization, and automation as
well as reduced use of energy, solvents, and toxic reagents. As
an example, in the next decade, SRC digestion approach, MIP-
AES, LC-ICP-MS, ICP-MSMS, and solid-sampling techniques
like XRF and LA-ICP-MS may be good candidates and
alternatives for multielemental determination in infant formula
and milk products.
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