Food

Elemental Analysis Manual (EAM) for Food and Related Products

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. 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 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.

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 or contributions 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

1. Regulatory Considerations

1.1 Program Areas (under development)

1.1.1 Chemical Contaminants
1.1.2 Food Labeling and Nutrition
1.1.3 Food Ingredients and Packaging

1.2 Regulatory Operations (Capar) (PDF, 333KB)

1.2.1 Regulatory Procedures Manual
1.2.2 Compliance Policy Guides manual
1.2.3 Compliance Program Guidance Manual
1.2.4 ORA Laboratory Manual
 

2. Sample Preparation

2.1 Food Edible Portion (Various) (PDF, 61KB)

2.1.1 General Procedures
2.2.2 Degasification of Carbonated Beverages

2.2 Food Homogenization (Mindak, Jacobs, Capar, Cunningham) (PDF, 214KB)

2.2.1 Laboratory Homogenization Equipment
2.2.2 Homogenization Procedures
2.2.2.1 General Procedures
2.2.2.2 Candy Procedures
2.2.2.3 Pills, Capsules, Supplements, etc.

2.3 Digestion and Separation (Mindak, Cheng, Capar) (PDF, 24KB)

2.3.1 Microwave Digestion (general applications)
2.3.2 References to Procedures in Various Methods
2.3.2.1 Leaching Cadmium and Lead from Ceramicware
2.3.2.2 Mercury Separation in Seafood
2.3.2.3 Arsenic Speciation in Rice

2.4 Contamination Control (Mindak, Capar) (PDF, 356KB)

2.4.1 Environmental
2.4.2 Laboratory Ware
 

3. General Analytical Operations and Information

3.1 Safety (Mindak) (PDF, 344KB)

3.2 Terminology (Cunningham, Mindak, Capar) (PDF, 413KB)

3.2.1 Figures of Merit
3.2.2 Samples and Sample Solutions
3.2.3 Standard Solutions
3.2.4 QC/QA Materials and Solutions

3.3 Uncertainty (Cunningham) (PDF, 555KB)

3.3.1 Types of Uncertainty
3.3.2 Sampling Uncertainty and Nonhomogeneity
3.3.3 Determining Analytical Uncertainty
3.3.4 Uncertainty on a Report of Analysis (under development)
3.3.5 Uncertainty and Method Development - Example for Method 4.4

3.4 Special Calculations (Capar, Mindak, Hight) (PDF, 114B)

3.4.1 Fortification Recovery
3.4.2 Other Recovery
3.4.3 Dilution Factor
3.4.4 Gravimetric Standard Solution Preparation
3.4.5 Percent Difference
3.4.6 Mass Correction Factor (MCF)

3.5 Reference Materials (Cunningham, Capar) (PDF, 468KB)

3.5.1 Reference Material Use For Quality Control
3.5.2 In-house Reference Material Development
3.5.2.1 Selection
3.5.2.2 Analytical
3.5.2.3 Random Error and Homogeneity
3.5.2.4 Uncertainties
3.5.2.5 Instructions
3.5.3 Reference Material Re-verification
3.5.4 Reference Material Sources
3.5.5 In-house Reference Material Certificates
3.5.5.1 FDA Cocoa Powder (CP)

3.6 Performance (Mindak, Cheng, Hight, Capar) (PDF, 567KB)

3.6.1 Instrument Performance
3.6.1.1 Graphite Furnace Atomic Absorption Spectrometer
3.6.1.2 Cold Vapor Atomic Absorption Spectrometer
3.6.1.3 Inductively Coupled Plasma-Atomic Emission Spectrometer
3.6.1.4 Inductively Coupled Plasma-Mass Spectrometer
3.6.2 Method Performance

3.7 Typical Element Concentrations (Capar, Cunningham) (PDF, 70KB)

4. Analytical Methods

4.1 Flame Atomic Absorption Spectrometric Determination of Lead and Cadmium Extracted from Ceramic Foodware (Hight)

4.2 Graphite Furnace Atomic Absorption Spectrometric Determination of Lead and Cadmium Extracted from Ceramic Foodware (Hight)

4.3 Graphite Furnace Atomic Absorption Spectrometric Determination of Cadmium and Lead in Food Using Microwave Assisted Digestion (Mindak, Cheng)

4.3A Appendix A – Supplemental Information on In-house Method Validation (Mindak, Cunningham)

4.3B Appendix B – Supplemental Information on Interlaboratory Trial (Mindak)

4.4 Inductively Coupled Plasma-Atomic Emission Spectrometric Determination of Elements in Food Using Microwave Assisted Digestion (Dolan, Mindak)

4.4A Appendix A – Supplemental Information on In-house Method Validation (Mindak, Capar)

4.4A Appendix A – Supplemental Information on In-house Method Validation - Table 4 (Mindak, Capar)

4.5 Cold Vapor Atomic Absorption Spectrometric Determination of Total Mercury in Seafood Using Microwave Assisted Digestion (Hight, Cheng)

4.5A Appendix A – Supplemental Information on In-house Method Validation (Cheng)

4.5B Appendix B – Supplemental Information on Method Performance (Cheng)

4.6 Inductively Coupled Plasma-Atomic Emission Spectrometric Determination of Cadmium and Lead Extracted from Ceramic Foodware (Cheng)

4.7 Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Lead and Mercury in Food Using Microwave Assisted Digestion (version 1.0; PDF, 683Kb) (Various)

4.8 High Pressure Liquid Chromatographic-Inductively Coupled Plasma-Mass Spectrometric Determination of Methylmercury and Total Mercury in Seafood (Cheng, Hight)

4.9 Portable Hand Held X-Ray Fluorescence Determination of Toxic Elements (under development)

4.10 High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination of Four Arsenic Species in Fruit Juice (version 0.82) (Conklin)

4.10 High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination of Four Arsenic Species in Fruit Juice (version 1.0; PDF, 443Kb) (Various)

4.11 Arsenic Speciation in Rice and Rice Products Using High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination (Various)


Glossary

TermDefinitionEAM Section
ASDLAnalytical Solution Detection Limit§3.2.1
ASQLAnalytical Solution Quantification Limit§3.2.1
CVAASCold Vapor-Atomic Absorption Spectrometry 
DFDilution Factor§3.4.3
FAPFortified Analytical Portion§3.2.4
FASFortified Analytical Solution§3.2.4
FMBFortified Method Blank§3.2.4
GFAASGraphite Furnace-Atomic Absorption Spectrometry 
ICPAESInductively Coupled Plasma-Atomic Emission Spectrometry 
ICPMSInductively Coupled Plasma-Mass Spectrometry 
ICSIndependent Check Solution§3.2.4
IDLInstrumental Detection Limit§3.2.1
LDRLinear Dynamic Range§3.2.1
LODLimit of Detection§3.2.1
LOQLimit of Quantification§3.2.1
MBKMethod Blank§3.2.4
MBKLLaboratory MBK§3.6.2
MBKCLaboratory MBK Critical Value §3.6.2
MCFMass Correction Factor§3.4.6
PDPercent Difference§3.4.5
RMReference Material§3.2.4
RPDRelative Percent Difference§3.4.5
RSDRelative Standard Deviation 
UAPUnfortified Analytical Portion 

 

Page Last Updated: 11/12/2014
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