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Annexe IV - Status of endorsement of methods of analysis and sampling

This Appendix consists of three sections:

Part I Methods of Analysis for Commodity Standards
Part II. Methods of Sampling for Commodity Standards
Part III. General Methods of Analysis
PART I. METHODS OF ANALYSIS FOR COMMODITY STANDARDS

COMMODITY

PROVISION

METHOD

PRINCIPLE

Note

Type

Status

A. Codex Committee on sugars

Sugars
(white sugar, plantation or mill white sugar, soft white sugar, soft brown sugar, powdered sugar, powdered dextrose, raw cane sugar)

Sulphur dioxide

ICUMSA GS 2-33 (1994)

Rosaniline procedure


III

E

Sugars
(powdered sugar)

Polarisation

ICUMSA (1994) GS 2/3-1

Polarimetry

Corrected reference to the method

II

E

Sugars
(fructose)

Conductivity ash

ICUMSA GS 2/3-17 (1994)

Conductimetry


I

E

Sugars
(soft sugars, brown sugar)

Invert sugar

ICUMSA GS 1/3/7-3

Titrimetry (Lane & Eynon)


I

E

Sugars
(plantation or mill white sugar)

Invert sugar

ICUMSA GS 2-6 (1998)

Titrimetry


I

E

Sugars
(soft white sugar, powdered sugar, plantation or mill white sugar)

Colour

ICUMSA GS 2/3-10 (1998)

Photometry

Corrected reference to the method. It was noted that the Commodity Committee recommended this method even though some members of the trade objected.

I

E

Honey

Sample preparation

AOAC 920.180



I


Honey

Moisture content

AOAC 969.38B
MAFF validated method V21

Refractometry

Both methods cited are identical

I

E

Honey

Fructose and Glucose (sum of both)

Harmonised method of the EHC, Apidologie, Special Issue 28, 1997, Chapter 1.7..2

HPLC

The Commodity Committee is requested to verify that a collaborative study has been performed on this method.

II

TE

Honey

Sucrose content

Harmonised method of the EHC, Apidologie, Special Issue 28, 1997, Chapter 1.7.2

HPLC

The Commodity Committee is requested to verify that a collaborative study has been performed on this method.

II

TE

Honey

Sugars added: for sugar profile

AOAC 998.18

Carbon isotope ratio mass spectrometry

AOACI has replaced method 991.41 with AOAC 998.18. It was also noted that at the last session method AOAC 978.17 was endorsed for honey (sugars added) and has been replaced with AOAC 998.12.

I

E

Honey

Water-insoluble solids content

MAFF validated method V22, J A Public Analyst 1992, 28(4) 189-193??

Gravimetry


I

E

Honey

Electrical conductivity

Harmonised method of the EHC, Apidologie, Special Issue 28, 1997, Chapter 1.2


The Commodity Committee is requested to verify that a collaborative study has been performed on this method.

I

TE

Honey

Acidity

MAFF Validated method V19, J A Public Analyst 1992, 28(4) 171-175.

Titrimetry


I

E

Honey

Diastase activity

Phadebas - Harmonised method of the EHC

Enzyme

The Commodity Committee is requested to verify that the reagents for the method are available, and a collaborative study has been performed on this method and to provide a method reference.

III

TE

Honey

Hydroxymethylfurfural

Harmonised method of the EHC

HPLC

The Commodity Committee is requested to verify that a collaborative study has been performed on this method and to provide a method reference.

III

TE

B. Codex Committee on Fish and Fishery Products

1. Methods referred back to CCCFFP

Quick Frozen Fish Sticks (fish fingers) and Fish Portions-Breaded and in Batter(except for certain fish species with soft flesh)

Proportion of fish fillet and minced fish

WEFTA Method

Gravimetry

The Commodity Committee is requested to provide the reference to the published method.

I

E

Quick Frozen Fish Sticks (fish fingers) and Fish Portions-Breaded and in Butter

Proportion of fish flesh in fish sticks
(fish core)

AOAC 996.15
(with an adjustment factor of 2% for raw breaded and batter-dipped products; 4% for precooked products)

Gravimetry

AOAC 996.15 is a modified method of AOAC 971.13 which was endorsed previously..

I

E

Salted Fish of the Gadidae Family

Salt

WEFTA Method

Titrimetry (Mohr)Salt determined as chloride expressed as sodium chloride

The Commodity Committee is requested to provide method reference.

II

E

2. Methods proposed in standards under elaboration

Fish and Fishery Products

Histamine

AOAC 977.13

Fluorimetry


II

E

C. Codex Committee on Milk and Milk Products

1. Methods of analysis referred back to CCMMP (adopted standards)

Cheese

Solids

IDF Standard 4A:1982
ISO 5534:1985

Gravimetry, drying at 102 C

The Working Group was interested in obtaining information on the difference in results between the previous method and this newly adopted method.

I

E

Cheese

Moisture

IDF Standard 4A:1982
ISO 5534:1985

Gravimetry, drying at 102°C

The Working Group was interested in obtaining information on the difference in results between the previous method and this newly adopted method.

I

E

Sweetened Condensed Milks

Solids

IDF Standard 15B:1991
ISO 6734:1989

Gravimetry, drying at 102 C

The Working Group was interested in obtaining information on the difference in results between the previous method and this newly adopted method.

I

E

Milkfat Products

Peroxide value (expressed as milliequivalents of oxygen/kg fat)

AOAC 965.33

Titrimetry


I

E

Evaporated Milks
Sweetened and Condensed Milks

Protein

AOAC 945.48H
AOAC 991.20 - IDF 20B:1993

Kjeldahl, titrimetry


I

E

Milkfat Products
Butter

Copper

IDF Standard 76A:1980/ISO 5738:1980/AOAC 960.40

Photometry, diethyldithiocarbamate

The Commodity Committee was encouraged to consider adopting one of the general methods for copper.

II

E

Whey Cheese

Dry matter (for denomination)

IDF Standard 58:1970 (confirmed 1993)
ISO 2920:1974

Gravimetry, drying at 88 C

.

I

E

Whey Powders

Lactose

IDF 79B:1991

Enzymatic method: glucose moiety (method A), galactose moiety (method B)


II

E

2. Methods of analysis proposed for standards under elaboration (advanced to Step 5 or 8)

Cheeses, individual

Dry matter
(specified in individual standards)

IDF Standard 4A:1982
ISO 5534:1985

Gravimetry, drying at 102°C

The Working Group was interested in obtaining information on the difference in results between the previous method and this newly adopted method

I

E

Cheeses, individual

Milkfat in dry matter

IDF Standard 5B:1986
ISO 1735:1987
AOAC 933.05

Gravimetry (Schmid-Bondzynski-Ratslaff)


I

E

Creams, Whipped Creams and Fermented Creams

Milk solids-not-fat

IDF Standard 80:1977
ISO 3727:1977
AOAC 920.116

Gravimetry


I

E

Creams, Whipped Creams and Fermented Creams

Milk solid-not-fat

IDF Standard 11A:1986

Gravimetry

The Commodity Committee should review to assure that this method is appropriate since the cited method is for milk solids in butter not cream.


NE

Cream

Milkfat

IDF Standard 16C:1987
ISO 2450:1999
AOAC 995.19

Gravimetry


I

E

Creams Lowered in Milkfat Content

Milkfat

IDF Standard 16C:1987
ISO 2450:1999
AOAC 995.19

Gravimetry


I

E

Edible Casein Products

Casein in protein

IDF Standard 29:1964

Titrimetry, Kjeldahl


I

E

Fermented Milks

Lactic acid

IDF Standard 150:1991
ISO 11869:1997

Potentiometry

The Commodity Committee should determine if the IDF method determines total acidity or lactic acid as in the provision.

I

NE

Fermented Milks

Lactic acid

AOAC 937.05

Spectrophotometric(for lactate acid in milk & milk products)

The Commodity Committee should clarify the provision or what type method they are requesting since there can’t be two type I or II methods.


NE

Fermented Milks

Protein

IDF Standard 20B:1993
AOAC 991.20-23

Titrimetry (Kjeldahl)


I

E

Fermented Milks

Dairy starter cultures of lactic acid bacteria (LAB)

IDF Standard 149A:1997
(Annex A)

Colony count at 25°C, 30°C, 37°C & 45°C according to the starter organism in question

The Commodity Committee should provide information on whether a collaborative study has been performed and the type of the method.

I

TE

Fermented Milks (Yoghurt)

Streptococcus thermophilus & Lactobacillus delbrueckii subsp. Bulgaricus
>= 107 cfu/g

IDF Standard 117B:1997

Colony count at 37°C

The Commodity Committee should provide information on whether a collaborative study has been performed and the type of the method.

I

TE

Fermented Milks (Yoghurt)

Streptococcus thermophilus & Lactobacillus delbrueckii subsp.bulgaricus
>= 107 cfu/g

IDF Standard 146A:1998

Test for identification

The Commodity Committee should provide information on whether a collaborative study has been performed and the type of the method.

I

TE

Milk Products obtained from Fermented Milks Heat-Treated after Fermentation

Protein

IDF Standard 20B:1993
ISO 8968 Part I
AOAC 991.20-23

Titrimetry (Kjeldahl)


I

E

Unripened Cheese Including Fresh Cheese1

Dry matter[not decided (unripened/fresh cheese)]
>= 35% (cream cheese)

IDF Standard 4A:1982
ISO 5534:1985

Gravimetry, drying at 102°C



NE

Unripened Cheese Including Fresh Cheese1

Dry matter
[not decided (unripened/fresh cheese)]
>= 35% (m/m), < Restricted by the MMFB

IDF Standard 4A:1982
ISO 5534:1985

Gravimetry, drying at 102 C



NE

Unripened Cheese Including Fresh Cheese1

Dry matter
[not decided (unripened/fresh cheese)]
>= 35% (cream cheese)

AOAC 926.08

Gravimetry, vacuum oven



NE

Unripened Cheese Including Fresh Cheese1

Protein

IDF Standard 20B:1993
AOAC 991.20-23
ISO 8968 Part I

Titrimetry, Kjeldahl


I

E

D. Codex Committee on Cocoa Products and Chocolate

Cocoa (Cacao) Mass, Cocoa/Chocolate (liquor) and Cocoa Cake

Fat content

AOAC 963.15 or IOCCC 14 (1972)

Sohxlet extraction


I

E

Cocoa powders (cocoas) and dry mixtures of cocoa and sugars

Cocoa butter

IOCCC 37 (1990) and IOCCC 14 (1972)

Total fat and total sterol content by GLC

The Commodity Committee is requested to provide evidence of collaborative study validation and information regarding the purpose and type of the method.


NE

Chocolate and Chocolate Products

Copper

NMKL 139
AOAC 971.20

Atomic absorption Spectrophotometry

The Commodity Committee should consider adopting one of the Codex general methods for copper that will handle the % fat in their product.


NE

E. Codex Coordinating Committee for Asia and Codex Committee on Processed Fruits and Vegetables

Aqueous Coconut Products

Total solids

AOAC 925.23A (IDF-ISO-AOAC method)

Gravimetry

AOAC 925.23kA has been repealed and the Commodity Committee should provide information on validation of the cited method for this application.

I

NE

Aqueous Coconut Products

Total Fats

AOAC 945.48G

Gravimetry (Röse-Gotlieb method)

The Commodity Committee should provide information on validation of the cited method for this application.

I

NE

F. Codex Committee on Soups and Broths

Soups and Broths

Creatinine

AIIBP Method 2/5 (2000)

HPLC


II

E

Soups and Broths

Creatinine

AOAC 920.115

Colorimetry

Based on the recommendation of the Commodity Committee this method should be deleted.


NE

Soups and Broths

Total Nitrogen

AOAC 928.08

Kjeldahl


II

E

Soups and Broths

Sodium Chloride

AIIBP No. 2/4

Potentiometric titration

Specification should be for chloride expressed as sodium chloride.

II

E

G. Codex Committee on Vegetable Proteins

Wheat Protein Products

Vital wheat gluten and devitalized wheat gluten

AOAC 979.09 (Wheat protein in grain N x 5.7)

Kjeldahl


I

E

Wheat Protein Products

Solubilized wheat protein

AOAC 920.87 (wheat protein in flour N x5.7)

Kjeldahl


I

E

H. Committee on Nutrition and Foods for Special Dietary Uses

Guidelines for Nutrition Labeling

Saturated fat

AOAC 996.06

Gas liquid chromatography


II

E

I. Codex Committee on Processed Fruits and Vegetables

Pickles

Benzoic acid

ISO 5518:1978

Spectrophotometry

The Commodity Committee is requested to review more modern methods such as the liquid chromatographic method IFU 63 (1995) or the gas chromatographic method NMKL 103 (1984)/AOAC 983.16 which has been endorsed as a Type II Codex general method.

IV

TE

Pickles

Lead

ISO 6633:1984

Flameless atomic absorption spectrophotometry


IV

TE

Pickles

Sorbates

ISO 5519:1978

Spectrophotometry

The Commodity Committee is requested to review more modern methods such as the liquid chromatographic method IFU 63 (1995) or the gas chromatographic method NMKL 103 (1984)/AOAC 983.16 which has been endorsed as a Type II Codex general method.

IV

TE

Pickles

Sulphur dioxide

ISO 5522:1981

Titrimetry followed by:
Gravimetry (high levels)
Nephelometry (low levels)

The Commodity Committee is requested to review the Optimized Monier-Williams method (AOAC 990.28), which has been endorsed as a Type II Codex general method.


NE

Pickles

Sulphur dioxide

ISO 5523:1981

Colorimetry

See above


NE

Pickles

Tin

ISO 2447:1998


The Commodity Committee is asked to consider whether it is necessary to express the provision using four significant figures.

IV

TE

1 The CCMMP decided to remove these provisions at their last session therefore method endorsement is unnecessary
PART II. METHODS OF SAMPLING FOR COMMODITY STANDARDS

A. Committee on Milk and Milk Products






Creams, Whipped creams and Fermented Creams Fermented Milks

Sampling

IDF Standard 50C:1995
ISO 707:1997
AOAC 968.12

General instructions

E


Sampling of Cheese in Brine
(Amendment at Step 3 of the Accelerated Procedure)

Amend Section 8.1 of the Codex Standard for Cheeses in Brine (CODEX STAN 208-1999) concerning sampling as follows (struck-out text to be deleted):

8.1 Sampling

According to IDF Standard 50C:1995/ISO 707:1997/AOAC 933.12. - Endorsed

Special requirements for cheese in brine: A representative piece of cheese is placed on a cloth or on a sheet of non-absorbent paper for 5 to 10 min. A slice of 2-3 cm is cut off and sent to the laboratory in a sealed insulated box for analysis.

B. Committee on Vegetable Proteins

Draft Standard for Wheat Protein Products

Sampling: ISO 13690: 1999 - Endorsed

PART III GENERAL CODEX METHODS

COMMODITY

PROVISION

METHOD

PRINCIPLE

Note

Type

Status

1. Methods for contaminants
All foods
Lead, cadmium, copper, iron and zinc
NMKL 139 (1991)
AOAC 999.11
AAS after dry ashing
Type II

II

E
All foods
Lead, cadmium, copper, iron and zinc
NMKL 161 (1998)
AOAC 991.10
AAS after microwave digestion
Type III

III

E
2. Methods for the detection of irradiated foods
Food containing fat
detection of irradiated food containing fat
EN 1784:1996
Gas chromatographic analysis of hydrocarbons


II

E
Food containing fat
detection of irradiated food containing fat
EN 1785:1996
Gas chromatographic(spectrophotometric analysis of 2/alkylcyclobutanones


III

E
Food containing bone
detection of irradiated food containing bones
EN 1786:1996
ESR spectroscopy


II

E
Food containing cellulose
detection of irradiated food containing cellulose
EN 1787:2000
ESR spectroscopy


II

E
Food from which silicate minerals can be isolated
detection of irradiated food from which silicate minerals can be isolated
EN 1788:1996
Thermoluminescence


II

E


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