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Appendix 4 - Laboratory Issues

Table of Contents | Part 1 | Part 2 | Appendix 1 | Appendix 2 | Appendix 3 | Appendix 4

Methods of Analysis

CFIA conducts laboratory tests to verify the accuracy of nutrition information. Methods of analysis currently used by the CFIA appear in the table below. The CFIA does not require other laboratories to use these methods. As improvements in methodology become available, these methods may be adopted at any time.

It is recommended that manufacturers engage laboratory testing to verify their own label declarations. The methods of analysis recommended are those published in the most recent version of the "Official Methods of Analysis of AOAC International" wherever possible. Other collaboratively studied methods such as those published by the American Oil Chemists' Society, American Association of Cereal Chemists, ISO, etc. would also be considered appropriate. In house or journal methods with adequate method validation data are another possible option for method selection. Methods should be validated for the food matrix being analyzed.

Laboratory Accreditation

Laboratories in Canada are accredited by the Standards Council of Canada and not by CFIA. Accredited laboratories will have a list of methods as part of their scope of accreditation. These methods are those considered by SCC during the accreditation process. When choosing accredited laboratories, the tests provided should be contained in their scope of accreditation. Laboratories should also strive to subscribe to proficiency testing schemes for each method listed in their scope.

Choice of Laboratory

CFIA recommends the selection of laboratories that are accredited to ISO 17025 standards by the Standards Council of Canada. CFIA cannot impose the use of only SCC accredited labs but recommends them as a first choice. ISO 17025 accredited laboratories from other countries would also be recommended. Company quality assurance laboratories using validated methods can also be used.

Table: Methods of Analysis used by CFIA - Nutrition Facts Table Core Information

Nutrient Method Reference Technique

Calories

 Atwater Method
(Guide to Food Labelling and Advertising, Chapter 6)

Application of appropriate factors to fat, carbohydrate (may be adjusted for sugar alcohols, polydextrose and known fibre source) and protein content
Fat
(Sum of fatty acids expressed as triglycerides)

AOAC 996.06*

Capillary Gas Chromatography using SP2560 100m x 0.25mm, 0.2µm film column

Fatty acids:

Saturates
(all fatty acids that contain no double bonds)

trans
( unsaturated fatty acids that contain one or more isolated or non-conjugated double bonds in trans configuration)

Monounsaturates
( cis monounsaturates)

Polyunsaturates
( cis methylene interrupted polyunsaturates)

  • Omega-3 polyunsaturates (s. B.01.001, FDR)
  • Omega-6 polyunsaturates (s.B.01.001,FDR)

AOAC 996.06*

Capillary Gas Chromatography using SP2560 100m x 0.25mm, 0.2µm film column

Cholesterol

AOAC 994.10*

Direct Saponification and Capillary Gas Chromatography
Carbohydrate
(mono- and di- saccharides + starch+ fibre+sugar alcohols+polydextrose)		 By Difference
(100-%ash-%moisture-%protein-%fat)

Determination by applicable AOAC method for: Ash, Moisture, Protein, and Fat

Fibre

AOAC 992.16* (Mongeau)

or

AOAC 985.29* (Prosky)

 Gravimetric determination after defatting and enzymatic hydrolysis of protein and carbohydrate (starch).
(Results found non-compliant by Mongeau method should be confirmed by Prosky method)
Sugars
(all monosaccharides and disaccharides)

AOAC 980.13* (modified HPLC column and mobile phase)

Aqueous food extraction followed by HPLC-RI

Protein

AOAC 981.10*
AOAC 993.13*

ISO 14891, Determination of Nitrogen Content using the Dumas Principle

Nitrogen by Kjeldahl or Combustion

Vitamin A
(retinol and derivatives and beta carotene expressed as retinol equivalents, RE)

AOAC 992.04*
(Méthod A-12 (version 3.0) 1993**)
Determination of Vitamin A in milk, infant formula, and other complex food commodities.

JAOAC. 76: nº 2, 1993
Method A-7**
HPLC Determination of Vitamin A in Margarine, Milk, Partially Skimmed Milk, and Skimmed Milk. JAOAC.63: 4, 1980

Method LPFC-200**
The fluorometric Determination of Vitamin A in Dairy products.
Journal of Dairy Sci,55:1077
(1992)

AOAC e-CAM #305, Determination of Beta and Alpha Carotene in Processed Foods

HPLC determination of vitamin A with UV detection

HPLC determination of vitamin A with UV detection

Fluorometric determination of vitamin A

Vitamin C
(L-ascorbic acid and L-dehydroascorbic acid and their derivatives, calculated as mg equivalents L-ascorbic acid)

HPLC-C1 (1992)**
Determination of vitamin C by HPLC.

Références:

1)Pelletier, O., And Brassard, R. Determination of Vitamin C in food by manual and automated methods. J. Food Sci., 42:1471-1477, 1977.

2)Behrens, W.A., and Madere, R.
Ascorbic and Dehydroascorbic acid content of infant formula.
J. Food Comp. Anal., 2: 48-52,1989.

3) Behrens, W. A., and Madere, R.
Ascorbic and Dehydroascorbic acid contents of canned food and frozen concentrated orange juice. J. Food Comp. Anal. 3: 3-8, 1990.

4) Behrens, W. A., and Madere, R. A Highly Sensitive High-Performance Liquid Chromatography Method for the Estimation of Ascorbic and Dehydroascorbic acid in Tissues, Biological Fluids, and Foods. Analytical Biochemistry 165:102-107, 1987.

5) J. Food Composition and Analysis V.11, p. 89-96, 1998, Electrochemical Determination of Ascorbic Acid and Isoascorbic Acid in Ground Meat and Processed Foods by HPLC.

HPLC determination of vitamin C with electrochemical detection

Iron

LPFC-137 **

Preparation of samples by calcination to determine different elements by atomic absorption flame spectroscopy

Calcium

LPFC-137**
AOAC 985.35*

Atomic Absorption Flame Spectroscopy
JAOAC 81, 1998, p1202 - 1208 Atomic Absorption Spectroscopy after Microwave Digestion
Sodium LPFC-137, as above**
LPFC-125**
A rapid method for the determination of sodium and potassium.
AOAC 969.23		 Preparation of samples by aqueous extraction or calcination and flame emission spectroscopy.

Iron, Calcium and Sodium

LCAQ-102 (Determination of Minerals in food by ICP-MS) Reference: Wu, S., Feng, X., and Wittmeir, A. Microwave Digestion of Plant and Grain Reference Materials in Nitric Acid or a Mixture of Nitric Acid and Hydrogen Peroxide for the Determination of Multi-elements by inductively Coupled Plasma Mass Spectrometry. Journal of Analytical Atomic Spectrometry 12:797-806, 1997 Reference: Dolan, S.P. and Capar, Stephen G. Multi-element Analysis of Food by Microwave Digestion and Inductively Coupled Plasma-Atomic Emission Spectrometry. Journal of Food Composition and Analysis 15:593-615, 2002.

Determination of minerals by ICP-MS after Microwave Digestion.

*Official Methods of Analysis of AOAC INTERNATIONAL(www.aoac.org) ed. W. Horowitz., AOAC INTERNATIONAL, Gaithersburg, Maryland, USA.

**available from CFIA or on Health Canada Web-site http://www.hc-sc.gc.ca/food-aliment/ns-sc/ne-en/labelling-etiquetage/e_nutrition_labelling_and_nutrie.html

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