APPENDIX V: METHODS OF ANALYSIS CONSIDERED BY THE COMMITTEE AT THE TWENTY-FIRST SESSION

This Appendix consists of four parts as follows:

Part 1. Methods of Analysis for Food Additives and Contaminants in Foods;
Part 2. Methods of Analysis for Commodity Standards Submittd for Endorsement;
Part 3. Amendment to the Previous Endorsement; and
Part 4. Methods of Analysis Temporarily Endorsed Previously

PART 1. METHODS OF ANALYSIS FOR FOOD ADDITIVES AND CONTAMINANTS IN FOODS

Commodity	Provision	Method	Principle	Note	Type	Status
Fats and oils	BHA, BHT, TBHQ, NDGA, propyl gallate	AOAC 983.15	Liquid chromatography		II	E
All foods	Cyclamates	NMKL 123 (1987)	Spectrophotometry	Collaborative study data on the NMKL methods were provided by the delegate from Finland.	II	E
Beverages and sweets	Saccharin	NMKL 122 (1987)	Liquid chromatography	See above.	II	E
All foods	Benzoic acid and its salt, sorbic acid and its salts	NMKL 103 (1984), AOAC 983.16	Gas chromatography	See above.	II	E
Cured meat	Nitrites	AOAC 973.31	Colorimetry	CEN and other groups have methods being developed for nitrites.	II	E
All foods	Sulphites >10 ppm sulphites	AOAC 990.28	Optimized Monier-Williams method	This method is recommended as Type II because of its wide acceptance and long history of use.	II	E
All foods	Sulphites >5 ppm total SO2	AOAC 990.29	Flow injection analysis		III	E
All foods	Sulphites >10 ppm SO2	AOAC 990.31	Ion exclusion chromatography		III	E

PART 2. METHODS OF ANALYSIS FOR COMMODITY STANDARDS SUBMITTED FOR ENDORSEMENT

A. Proposed by Codex Committee on Fats and Oils

Commodity	Provision	Method	Principle	Note	Type	Status
Fats and Oils	Acidity <10 mg-KOH/g	IUPAC 2.201 ISO 660:1996	Titrimetry		I	E
Palm Oil	Apparent density 0.8813-0.8977	ISO 6883:1995 with the appropriate conversion factor	Pyknometry		I	E
Fats and Oils	Arsenic <0.1 mg/kg	AOAC 942.17 (Codex general method)	Colorimetry (molybdenum blue)		III	E
Fats and Oils	Arsenic <0.1 mg/kg	AOAC 952.13 (Codex general method) IUPAC 3.136	Colorimetry (diethyldithocarbamate)		II	E
Fats and Oils	Arsenic <0.1 mg/kg	AOAC 985.16 (Codex general method)	Atomic absorption spectrometry		III	E
Fats and Oils	Baudouin test (modified Villavecchia or sesameseed oil test) +/-	AOCS Cb 2-40	Colour reaction		I	E
Fats and Oils	Copper and Iron <0.1 mg/kg	ISO 8294:1994 IUPAC 2.631 AOAC 990.05 (Codex general method)	Atomic absorption spectrometry (direct graphite furnace)		II	E
Fats and Oils	Crismer value 67-70	AOCS Cb 4-35	Turbidity		I	E
Fats and Oils	Fatty acid composition various levels	IUPAC 2.301+2.302+2.304, ISO 5509:1978+5508:1990	Gas chromatography of methyl esters		II	E
Fats and Oils	Halphen test +/-	AOCS Cb 1-25	Colorimetry		I	E
Fats and Oils	Insoluble impurities 0.05-0.1% (m/m)	IUPAC 2.604 ISO 663:1995	Gravimetry		I	E
Fats and Oils	Iodine value 6.3-148 % m/m absorbed iodine	AOCS Cd 1b-1987	Calculation from the fatty acid profile	The Commodity Committee (CC) is requested to specify the oils that each method is applicable to.	I	TE
Fats and Oils	Iodine value 6.3-148 % m/m absorbed iodine	IUPAC 2.205/1 ISO 3961:1996 AOAC 993.20 AOCS Cd 1d-1992	Wijs-titrimetry	The Commodity Committee (CC) is requested to specify the oils that each method is applicable to.	I	TE
Fats and Oils	Iron 1.5-3.0 mg/kg	ISO 8294:1994 IUPAC 2.631 AOAC 990.05 (Codex general method)	Atomic absorption spectrometry (direct graphite furnace)		II	E
Fats and Oils	Lead <0.1 mg/kg	IUPAC 2.632 AOAC 994.02 ISO 12193:1994 (Codex general method)	Atomic absorption (direct graphite furnace)		II	E
Fats and Oils	Matter volatile at 105°C <0.3% (m/m)	IUPAC 2.601 ISO 662:1996	Gravimetry (open-drying)		I	E
Fats and Oils	Peroxide value 0-20 meq-active oxygen/kg	IUPAC 2.501 (as amended) AOCS Cd 8b-90	Titrimetry using iso-octane		I	E
Fats and Oils	Refractive index 1.447-1.470	IUPAC 2.102 ISO 6320:1995	Refractometry		II	E
Fats and Oils	Reichert & Polenske values 6-8.5 (Reichert value) 8-18 (Polenske value)	IUPAC 2.204	Tritrimetry		I	E
Fats and Oils	Relative density 0.881-0.927	IUPAC 2.101	Pyknometry		II	E
Fats and Oils	Saponification value 168-265 mg-KOH/g-oil	IUPAC 2.202 ISO 3657:1988	Titrimetry		I	E
Fats and Oils	Slip point	ISO 6321:1991	Open ended capillary tube		I	E
Palm oil	Slip point 24-44°C for palm oil	AOCS Cc 3-25 (1992)	Open ended capillary tube (for 60°C)		I	E
Fats and Oils	Soap content 0.005% (m/m)	BS 684 Section 2.5	Gravimetry		I	E
Fats and Oils	Sterol composition -	ISO 6799:1991 IUPAC 2.403	Gas chromatography		II	E
Fats and Oils	Titre 32-49°C	IUPAC 2.121 ISO 935:1988	Thermometry		I	E
Fats and Oils	Tocopherol composition -	IUPAC 2.432	HPLC	ISO/DIS reference was deleted. When the final method reference becomes available its inclusion will be considered.	II	E
Fats and Oils	Total carotenoids 300-2000 mg-b-carotene/kg	BS 684 Section 2.20	Spectrophotometry		II	E
Fats and Oils	Unsaponifiable matter 0-30 g/kg	IUPAC 2.401 (part 1-5) ISO 3596-1:1996	Titrimetry after extraction with diethyl ether		I	E

B. Proposed by Codex Committee on Sugars

Commodity	Provision	Method	Principle	Note	Type	Status
Honey	Acidity <40 meq-acid/kg	J. Assoc. Public Analysts (1992) 28 (4) 171-175 MAFF Validated V19 for Acidity in Honey			I	E
Sugars (lactose)	Anhydrous lactose >99.0%	ICUMSA GS 4/3-3 (1994)	Titrimetry		II	E
Sugars (powdered sugar)	Anti-caking agents <1.5% m/m	ICUMSA GS 3-21 (1994) to be amended to incorporate a method for the determination of starch to meet the requirements of the Standard		ICUMSA is requested to provide needed information on methods and the status of collaborative studies.		NE
Honey	Apparent reducing sugar >45%	Stated in the Standard (Annex 2 of CX/MAS 97/9)	Titrimetry (Lane & Eynon)		I	E
Honey	Apparent sucrose <10%	FAO Manuals of Food Quality Control, Food and Nutrition Monograph 14/3 (1979) 150	Walker Inversion		I	E
Honey	Arsenic free from As	AOAC 952.13 (Codex general method)	Colorimetry (diethyldithiocarbamate)	The CC should provide a quantitative provision for As rather than "free from As". It was assumed that the <1 mg/kg As in the sugars specification would be adequate for method sensitivity.	II	E
Sugars	Arsenic <1 mg/kg	AOAC 952.13 (Codex general method)	Colorimetry (diethyldithiocarbamate)		II	E
Sugars	Arsenic <1 mg/kg	ICUMSA GS 2/3-25 (1994)	Colorimetry (diethyldithiocarbamate)	If this method is identical to AOAC 952.13, it should be put together with the AOAC method.	IV	TE
Sugars (soft white sugar and soft brown sugar)	Colour -	ICUMSA GS 1-7 (1994)	Photometry		I	E
Sugars (powdered sugar)	Colour <60 ICUMSA units	ICUMSA GS 2/3-9 (1994)	Photometry		I	E
Sugars (plantation or mill white sugar, soft white sugar and soft brown sugar)	Conductivity ash <0.2% m/m	ICUMSA GS 1/3/4/7/8-13 (1994)	Conductimetry y		I	E
Sugars (white sugar)	Conductivity ash <0.04% m/m	ICUMSA GS 2/3-17 (1994)	Conductimetry		I	E
Sugars (powdered sugar)	Conductivity ash <0.04% m/m	ICUMSA GS 2/3-17 (1994)	Conductimetry		I	E
Honey	Copper free from Cu	AOAC 971.20 (Codex general method)	Atomic absorption spectrophotometry	The CC should specify a quantitative level of Cu for the provision so CCMAS can be sure the method is adequately sensitive.	II	E
Sugars (dextrose anhydrous, dextrose monohydrate)	D-glucose >99.5% m/m on a dry basis	ISO 5377:1981	Titrimetry		I	E
Honey	Diastase activity >3	AOAC 958.09	Photometry		II	E
Honey	Diastase activity >3	Stated in the Standard (CX/MAS 97/9-Add.1) Other commercially available calibrated substrate preparations can also be used.	Photometry	Use of a proprietary reagent in the method requires the change noted in the principle section.	III	E
Honey	hydroxymethylfurfural <80 mg/kg	AOAC 980.23	Spectrophotometry		II	E
Honey	hydroxymethylfurfural <80 mg/kg	Stated in the Standard (CX/MAS 97/7-Add.1)	HPLC		III	E
Honey	hydroxymethylfurfural <80 mg/kg	Stated in the Standard (CX/MAS 97/7-Add.1)	Photometry (Winkler)	This method uses p-toluidine which is carcinogenic.	III	E
Sugars (plantation or mill white sugar)	Invert sugar <0.1% m/m	ICUMSA GS 1/3/7-3 (1994)	Titrimetry (Lane & Eynon)		I	E
Sugars (soft white sugar and soft brown sugar)	Invert sugar 0.3-12.0% m/m	ICUMSA GS 1/3/7-3 (1994)	Titrimetry (Lane & Eynon)		I	E
Sugars (white sugar)	Invert sugar <0.04% m/m	ICUMSA GS 2/3-5 (1997)	Titrimetry		I	E
Sugars (powdered sugar)	Invert sugar <0.04% m/m	ICUMSA GS 2/3-5 (1997) after filtration if necessary to remove any anticaking agents	Titrimetry		I	E
Honey	Lead free from Pb	AOAC 972.25 (Codex general method)	Atomic absorption spectrophotometry	The CC should specify a quantitative level of Pb for the provision so CCMAS can be sure the method is adequately sensitive.	II	E
Honey	Lead free from Pb	Miller-Ihli method (JAOAC International(1994) 77(5), 1288-1292)		The method was not endorsed because it had no collaborative study data submitted and no official AOAC International status.		NE
Sugars	Lead <0.5 mg/kg	AOAC 972.25 (Codex general method)	Atomic absorption spectrophotometry		II	E
Sugars	Lead <0.5 mg/kg	Miller-Ihli method (JAOAC International (1994) 77(5) 1288-1292)		The method was not endorsed because it had no collaborative study data submitted and no official AOAC International status.		NE
Sugars (lactose)	Loss on drying <6.0% m/m	USP method (1995)	Gravimetry (drying at 120°C for 16 h)	Previous reference: CAC/RM 2-1969.	I	E
Sugars (soft white sugar, soft brown sugar, white sugar, plantation or mill white sugar and powdered sugar)	Loss on drying <4.5% m/m	ICUMSA GS 2/1/3-15 (1994)	Gravimetry		I	E
Sugars (fructose)	Loss on drying <0.5% m/m	ISO 1742:1980	Gravimetry		I	E
Honey	Mineral (ash) <1.0%	J. Assoc. Public Analysts (1992) 28 (4) 177-181 MAFF Validated Method V20 for Mineral (ash) in Honey	Gravimetry (ignition at 600°C)		I	E
Honey	Moisture <23%	AOAC 969.38B J. Assoc. Public Analysts (1992) 28 (4) 183-187 MAFF Validated Method V21 for Moisture in Honey	Refractometry		I	E
Sugars (fructose and lactose)	pH 4.5-7.0	ICUMSA GS 1/2/3/4/7/8-23 (1994)	Potentiometry		I	E
Sugars (plantation or mill white sugar)	Polarization >99.5°Z	ICUMSA GS 1/2/3-1 (1994)	Polarimetry		II	E
Sugars (white sugar)	Polarization >99.7°Z	ICUMSA GS 2/3-1 (1994)	Polarimetry		II	E
Sugars (powdered sugar)	Polarization >99.7°Z	ICUMSA GS 2/3-1 after filtration in necessary to remove any anti-caking agents	Polarimetry		II	E
Sugars (dried glucose syrup and glucose syrup)	Reducing sugar >20.0% m/m on a dry basis expressed as D-glucose	ISO 5377:1981	Titrimetry		I	E
Honey	Sample preparation	AOAC 920.180	-	The Committee proposed to use AOAC 920.180 as it is identical to the method currently stated in the Standard and to change the provision from sampling to sample preparation.	-	E
Sugars (fructose)	Specific rotation -89° - -93.5°	Zuckerindustrie 113 (1988); 1, 49-50	Polarimetry	Status retained pending further information.	II	TE
Sugars (soft white sugar and soft brown sugar)	Sucrose plus invert sugar >88.0% m/m expressed as sucrose	ICUMSA GS 4/3-7 (1994)	Titrimetry		I	E
Sugars (soft white sugar and soft brown sugar)	Sulphated ash <3.5% m/m	ICUMSA GS 1/3/4/7/8-11 (1994)	Gravimetry		I	E
Sugars (lactose)	Sulphated ash <0.3% m/m on a dry basis	ICUMSA GS 1/3/4/7/8-11 (1994)	Gravimetry		I	E
Sugars (dextrose anhydrous, dextrose monohydrate, dried glucose syrup and glucose syrup)	Sulphated ash <1.0% m/m on a dry basis	ISO 5809:1982	Single sulphonation		I	E
Sugars (powdered dextrose)	Sulphated ash <0.25% m/m on a dry basis	ISO 5801		The Committee was informed of the proposal to use ISO 5801 but postponed discussions pending the information on the ISO method.
Sugars (white sugar and plantation or mill white sugar)	Sulphur dioxide <20 mg/kg	ICUMSA GS 2/7-33 (1994)	Colorimetry	The CC Secretariat should provide clarification of ICUMSA method numbers, collaborative study data and clarification concerning applicability of
Sugars (white sugar and plantation or mill white sugar)	Sulphur dioxide <20 mg/kg	ICUMSA GS 2/3-35 (1994)	Enzymatic method	both sulphur dioxide methods to powdered sugar with and without anti-caking agents.
Sugars (powdered sugar without anti-caking agents)	Sulphur dioxide <15 mg/kg	ICUMSA GS 2/7-33 (1994)	Colorimetry	See above and only listed as applicable for white sugar in ICUMSA methods book.
Sugars (powdered sugar without anti-caking agents)	Sulphur dioxide <15 mg/kg	ICUMSA GS 2/3-35 (1994)	Enzymatic method	.
Sugars (powdered sugar with anti-caking agents)	Sulphur dioxide <15 mg/kg	ICUMSA GS 2/3-35 (1994)	Enzymatic method	The CC Secretariat should confirm that the colorimetric method is not applicable to this commodity.
Sugars (dextrose anhydrous, dextrose monohydrate, glucose syrup, dried glucose syrup and fructose)	Sulphur dioxide <20 mg/kg	ISO 5379:1983	Acidimetry and nephelometry		IV	TE
Sugars (dextrose anhydrous and dextrose monohydrate)	Total solids >90.0% m/m	ISO 1741:1980	Gravimetry (vacuum oven)		I	E
Sugars (dried glucose syrup and glucose syrup)	Total solids >70.0% m/m (glucose syrup) >93.0% m/m (dried glucose syrup)	ISO 1742:1980	Gravimetry (vacuum oven)		I	E
Honey	Water-insoluble solids <0.5%	J. Assoc. Public Analysts (1992) 28 (4) 189-193 MAFF Validated Method V22 for Water-Insoluble Solids in Honey	Gravimetry		I	E

C. Proposed by the Codex Committee on Fish and Fishery Products

Commodity	Provision	Method	Principle	Note	Type	Status
Quick Frozen Fish Sticks (Fish Fingers)	Proportion of fish fillet/minced fish flesh not specified	Stated in the Standard (Annex 3 of CX/MAS 97/9)	Gravimetry	No decision was made pending submission of UK collaborative study data.
Salted Fish and Dried Salted Fish of the Gadidae Family	Salt not specified	Stated in the Standard (Annex 4 of CX/MAS 97/9)	Titrimetry (Mohr)	The CC should be requested to consider the General Method for Salt AOAC 971.27 instead of the proposed method and questioned whether a method was needed since no specification was listed.

D. Proposed by the Codex Coordinating Committee for Asia

Commodity	Provision	Method	Principle	Note	Type	Status
Canned Bamboo Shoot	Colour, flavour, texture	Stated in the Standard (Annex 5 of CX/MAS 97/9)	Organoleptic measurement	The CC Secretariat should be informed that items such as organoleptic measurements of colour, flavour and texture are not ordinarily considered as methods of analysis.		NE
Canned Bamboo shoot	Net weight and drained weight drained wt/net wt>60%	AOAC 968.30	Gravimetry	CC should be informed that WG endorsed the AOAC method which appears to be identical to the method stated in the Standard (Annex 6 of CX/MAS 97/9).	I	E
Canned Bamboo Shoot	pH >4.0; 4.0-4.6 (if acid is added)	AOAC 981.12	Potentiometry		I	E
Dried Salted Anchovies	Acid insoluble ash <1.5% m/m (dry basis)	Stated in the Standard (Annex 7 of CX/MAS 97/9)	Gravimetry	It was recommended that the CC consider adopting a more generally applicable method such as AOAC 938.08.
Dried Salted Anchovies	Sodium chloride <15% m/m (dry basis)	AOAC 937.09	Volumetry		II	E
Dried Salted Anchovies	Water activity <0.75	AOAC 978.18 or methods using any instruments equivalent to the instruments described in AOAC 978.18	Measurement of vapour pressure, dew point or physical or electric characteristics of sensors using instruments		I	E
Fish Crackers	Crude protein (Nx6.25) >5% m/m	AOAC 920.87	Titrimetry (Kjeldahl)		I	E
Fish Crackers	Crude protein (Nx6.25) >2% m/m	AOAC 960.52	Titrimetry (micro-Kjeldahl)	CC should be requested to consider the more general method AOAC 920.87 given potential sampling problems and that method 960.52 has been surplused by AOAC.
Fish Crackers	Moisture 8-14% m/m	AOAC 950.46B	Gravimetry (air-drying)	CC needs to select one of the two drying conditions specified in the method or provide data indicating their comparability.

APPENDIX III

PART 3. AMENDMENT TO THE PREVIOUS ENDORSEMENT

Commodity	Provision	Method	Principle	Note	Type
Processed Meat and Poultry Products and Soups and Broths	Nitrite	ISO 2918:1975	Colorimetry	Previously endorsed as Type II. Reclassification recommended based on the lack of collaborative study data.	IV

APPENDIX IV

PART 4. METHODS OF ANALYSIS TEMPORARILY ENDORSED PREVIOUSLY

1. The Committee extended the temporarily endorsed status of the following methods.

Commodity	Provision	Method	Principle	Note	Type
Edible cassava flour	Ash < 3 % (m/m)	AOAC 923.03	Gravimetry	It was proposed to extend the temporary endorsement of AOAC 923.03 working at 550°C and requested the ISO information on the temperature used in ISO 2171:1993 whether it is only 900°C. CC should be contacted concerning the necessary oven temperature.	I
Grated desiccated coconut	Granularity Extra fine, fine and medium	ISO 2591-1:1988 Test Sieving According to British Standard Mesh Nominal Test Sieves: BS 410-1986	Sieving		I
Guidelines for nutrition labelling	Polyunsaturated fat	AOCS Ce 1c-89	Gas liquid chromatography	It was noted that AOAC 996.06 became available and the method should be submitted to the CCNFSDU for consideration.	IV
Guidelines for nutrition labelling	saturated fat	AOCS Ce 1c-89	Gas liquid chromatography	It was noted that AOAC 996.06 became available and the method should be submitted to the CCNFSDU for consideration.	IV

2. The Committee replaced the previously proposed method with the following method with temporary endorsement.

Commodity	Provision	Method	Principle	Note	Type
Durum wheat semolina and durum wheat flour	Particle size	AFNOR NFV 03721	Sieving	It was proposed to temporarily endorse the AFNOR method with the understanding that when it is finalized as an ISO method, it will be replaced by the ISO method reference.	I