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U.S. Department of Health and Human Services

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Elemental Analysis Manual (EAM)

for Food and Related Products

Send comments or contributions to
EAM@fda.hhs.gov

periodic table with B, Na, Mg, Al, P, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Sr, Mo, CD, Ba, Hg, Tl, and Pb highlighted

The U. S. Food and Drug Administration's (FDA) responsibility for maintaining a safe food supply is met in part by monitoring for toxic and nutritional elements in food and related products. FDA collects and analyzes food and foodware from commercial channels of trade for determining regulatory compliance. Analytical data gathered under these monitoring activities are also used for evaluating the extent and significance of these analytes in the food supply.

The Elemental Analysis Manual (EAM) for Food and Related Products provides a repository of the analytical methods used in FDA laboratories to examine food for toxic and nutrient elements for regulatory purposes. The manual also provides general guidance on related aspects of a laboratory analysis.

Introduction

An FDA Elemental Analysis Manual (EAM) was produced in 1982 as an internal document for FDA laboratories. The manual was a compilation of published analytical methods and procedures commonly used at that time by FDA analysts, as well as comments based on the experiences of these analysts in using the methods. The EAM served as a source of information to help standardize the way elemental analyses were conducted in FDA laboratories.

The current online version of the EAM is intended to provide FDA laboratories a source of current information and laboratory procedures for determining the level of toxic and nutrient elements in food and related products. The analytical methods in the EAM are based on published peer reviewed analytical procedures that have been expanded to include our experiences on improving the quality of the analyses. The EAM does not contain all procedures that may be used by FDA laboratories. Another source of procedures used by FDA is the Official Methods of Analysis of AOAC INTERNATIONAL disclaimer icon. In addition, compliance programs issued by FDA may have specific analytical instructions and FDA field laboratories use a Laboratory Manual that provides guidance on primary laboratory functions. New analytical procedures will be added to the EAM when they are validated and routinely used by FDA laboratories.

Text for the EAM was peer-reviewed by FDA laboratory scientists in the Center for Food Safety and Applied Nutrition and the Office of Regulatory Affairs. An Elemental Analysis Steering Committee composed of FDA laboratory scientists will maintain the EAM. Sections of the EAM will be added or revised based on their recommendations.

The analytical methods in Section 4 have at least completed a single laboratory validation and are based on analytical procedures that have been published in peer reviewed scientific journals. Some of the EAM methods are based on methods that have successfully completed a multilaboratory study. All methods will complete a single laboratory validation before being listed in the EAM followed by at least an FDA interlaboratory trial. Documentation of the extent of validation is presented as a supplement to the method and will be expanded as additional validation studies are completed.

The EAM is only available through the Internet.

When referring to an EAM method or section the revision number should be included. The following is a suggested format for citing an EAM method:

FDA Elemental Analysis Manual [Internet]. College Park (MD): Food and Drug Administration (US), Center for Food Safety and Applied Nutrition; Section 4.3 [Version 1; 2008 June]. Graphite Furnace Atomic Absorption Spectrometric Determination of Cadmium and Lead in Food Using Microwave Assisted Digestion. Available from:
http://www.fda.gov/EAM (Accessed 2011 November 2).

Send comments to EAM@fda.hhs.gov

The mention of specific items of equipment and chemicals by brand name or the supplying of manufacturer's names and addresses do not constitute endorsement of a product or source by the United States Government.


 

Table of Contents

SectionTitleAuthor(s)
1Regulatory Considerations 
1.1Program Areas{Under Development}
1.1.1Chemical Contaminants 
1.1.2Food Labeling and Nutrition 
1.1.3Food Ingredients and Packaging 
1.2Regulatory OperationsS.G. Capar
1.2.1Regulatory Procedures Manual 
1.2.2Compliance Policy Guides Manual 
1.2.3Compliance Program Guidance Manual 
1.2.4ORA Laboratory Manual 
2Sample Preparation 
2.1Laboratory Sample to Analytical SampleS.G. Capar
K. Egan
R.M. Jacobs
2.1.1Food Edible Portion 
2.1.2Candy Preparation 
2.1.3Carbonated Beverage Degasification 
2.2Analytical Sample to Analytical PortionS.G. Capar
R.M. Jacobs
2.2.1Homogenization Equipment 
2.2.2Homogenization Procedures 
2.3Analytical Portion to Analytical SolutionW.R. Mindak
J. Cheng
R.M. Jacobs
2.3.1Microwave Digestion 
3General Analytical Operations and Information 
3.1Contamination ControlW.R. Mindak
S.G. Capar
3.1.1Environmental 
3.1.2Laboratory Ware 
3.2Analytical Figures of MeritS.G. Capar
W.C. Cunningham
3.2.1Instrument 
3.2.2Analytical Solution 
3.2.3Analytical Portion 
3.3UncertaintyW.C. Cunningham
3.3.1Uncertainty Calculations 
3.3.2Determination of a Specific Uncertainty 
3.3.3Special Situations and Nonhomogeneity 
3.3.4Consistency with the ORA Laboratory Manual 
3.4Special CalculationsS.G. Capar
W.R. Mindak
S.C. Hight
3.4.1Fortification Recovery 
3.4.2Other Recovery 
3.4.3Dilution Factor 
3.4.4Gravimetric Standard Solution Preparation 
3.4.5Percent Difference 
3.4.6Mass Correction Factor 
3.5Reference MaterialsW.C. Cunningham
S.G. Capar
3.5.1Reference Material Use for Quality Control 
3.5.2In-house Reference Material Development 
3.5.3Reference Material Re-verification 
3.5.4Organizations Providing Reference Materials 
3.5.5Compilation of Sources of Reference Materials 
3.5.6In-House Reference Material Certificates 
3.6Instrument Performance 
3.6.1Graphite Furnace Atomic Absorption SpectrometerW.R. Mindak
3.6.2Cold Vapor Atomic Absorption SpectrometerJ. Cheng
S.C. Hight
3.6.3Inductively Coupled Plasma-Atomic Emission SpectrometerW.R. Mindak
J. Cheng
3.6.4Inductively Coupled Plasma-Mass SpectrometerW.R. Mindak
3.7Typical Element ConcentrationsS.G. Capar
3.7.1U. S. Food and Drug Administration 
3.7.2U. S. Department of Agricultural 
3.7.3Food Standards Agency (United Kingdom) 
3.7.4Food Standards Australia New Zealand 
3.7.5Health Canada 
4Analytical Methods 
4.0.1TerminologyS.G. Capar
4.0.2Method Performance ChecksS.G. Capar
W.R. Mindak
W.C. Cunningham
4.0.3SafetyW.R. Mindak
4.1Flame Atomic Absorption Spectrometric Determination of Lead and Cadmium Extracted from Ceramic FoodwareS.C. Hight
4.2Graphite Furnace Atomic Absorption Spectrometric Determination of Lead and Cadmium Extracted from Ceramic FoodwareS.C. Hight
4.3Graphite Furnace Atomic Absorption Spectrometric Determination of Cadmium and Lead in Food Using Microwave Assisted DigestionW.R. Mindak
J. Cheng
4.3AAppendix A – Supplemental Information on In-house Method ValidationW.R. Mindak
W.C. Cunningham
4.3BAppendix B – Supplemental Information on Interlaboratory TrialW.R. Mindak
4.4Inductively Coupled Plasma-Atomic Emission Spectrometric Determination of Elements in Food Using Microwave Assisted DigestionS.P. Dolan
W.R. Mindak
4.4AAppendix A – Supplemental Information on In-house Method ValidationW.R. Mindak
S.G. Capar
4.5Cold Vapor Atomic Absorption Spectrometric Determination of Total Mercury in Seafood Using Microwave Assisted DigestionS.C. Hight
J. Cheng
4.5AAppendix A – Supplemental Information on In-house Method ValidationJ. Cheng
S.C. Hight
4.5BAppendix B – Supplemental Information on Method PerformanceJ. Cheng
4.6Inductively Coupled Plasma-Atomic Emission Spectrometric Determination of Cadmium and Lead Extracted from Ceramic FoodwareJ. Cheng
4.7Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Lead and Mercury in Food Using Microwave Assisted Digestion (version 1.0; PDF, 683Kb)Patrick J. Gray
William R. Mindak
John Cheng
4.8High Pressure Liquid Chromatographic-Inductively Coupled Plasma-Mass Spectrometric Determination of Methylmercury and Total Mercury in SeafoodJ. Cheng
S.C. Hight
4.9Portable Hand Held X-Ray Fluorescence Determination of Toxic Elements{Under Development}
4.10High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination of Four Arsenic Species in Fruit Juice (version 1.0; PDF, 443Kb)S.D. Conklin
K.M. Kubachka
N.V. Shockey
4.11Arsenic Speciation in Rice and Rice Products Using High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric DeterminationK.M. Kubachka
N.V. Shockey
T.A. Hanley
S.D. Conklin
D.T. Heitkemper

 

Glossary

TermDefinitionEAM Section
ASDLAnalytical Solution Detection Limit§3.2.2
ASQLAnalytical Solution Quantification Limit§3.2.2
CVAASCold Vapor-Atomic Absorption Spectrometry 
DFDilution Factor§3.4.3
FAPFortified Analytical Portion§3.4.1, §4.0.1.3, §4.0.2.2
FASFortified Analytical Solution§3.4.1, §4.0.1.3, §4.0.2.3
FMBFortified Method Blank§4.0.1.3, §4.0.2.4
GFAASGraphite Furnace-Atomic Absorption Spectrometry 
ICPAESInductively Coupled Plasma-Atomic Emission Spectrometry 
ICPMSInductively Coupled Plasma-Mass Spectrometry 
ICSIndependent Check Solution§4.0.1.3
IDLInstrumental Detection Limit§3.2.1
LDRLinear Dynamic Range§3.2.1
LODLimit of Detection§3.2.3
LOQLimit of Quantification§3.2.3
MBKMethod Blank§4.0.1.3
MBKLLaboratory MBK§4.0.2.5
MBKCLaboratory MBK Critical Value§4.0.2.6
MCFMass Correction Factor§3.4.6
PDPercent Difference§3.4.5
RMReference Material§3.4.2, §3.5
RPDRelative Percent Difference§3.4.5
RSDRelative Standard Deviation 
UAPUnfortified Analytical Portion