ALINORM 04/27/23
APPENDIX VI
STATUS OF ENDORSEMENT OF METHODS OF ANALYSIS AND SAMPLING
Part I. METHODS OF ANALYSIS
A. Codex Committee on Fats and Oils
B. Codex Committee on Fish and Fishery Products
C. Ad hoc Intergovernmental Task Force on Fruit and Vegetable Juices
D. Codex Committee on Nutrition and foods for special dietetary uses
E. Methods of Analysis for Additives and Contaminants
A. CODEX COMMITTEE ON FATS AND OILS1
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
NOTE |
TYPE |
STATUS |
Fat Spreads and Blended Spreads |
Milk fat content (butyric acid) |
IUPAC 2.310, AOAC 990.27 or AOCS Ca 5c-87 (97). |
Saponification, acidification, water soluble fatty acid separation, GLC determination |
CCFO should determine a conversion factor |
I |
TE |
Olive Oils and Olive Pomace Oils |
Organoleptic characteristics |
COI/T.20/Doc. no. 15. |
Panel test |
I |
E | |
Free acidity (acid value) |
ISO 660:1996, amended 2003 or
|
Titrimetry |
I |
E | ||
Fatty acid composition |
COI/T.20/Doc. no. 24 and ISO 5508: 1990 and AOCS Ch 2-91(02) or AOCS Ce 1f-96 (02)
|
Gas chromatography of methyl esters |
II |
E | ||
Trans fatty acids content |
COI/T.20/Doc no. 17 or ISO 15304:2002 or AOCS Ce 1f-96 (02) |
Gas chromatography of methyl esters |
II |
E | ||
Wax content |
COI/T.20/Doc. no. 18 or AOCS Ch 8-02 (02) |
Gas chromatography |
II |
E | ||
Difference between the actual and theoretical ECN 42 triglyceride content |
COI/T.20/Doc. no. 20 or AOCS Ce 5b-89 (97) |
Analysis of triglycerides of HPLC and calculation |
I |
E | ||
Sterol composition and total sterols |
COI/T.20/Doc. no. 10 or ISO 12228:1999 or AOCS Ch 6-91 (97). |
Gas chromatography |
II |
E | ||
Erythrodiol + uvaol content |
IUPAC 2.431. |
Gas chromatography |
II |
E | ||
Stigmastadienes |
COl/T.20/Doc. no. 11 or ISO 15788-1:1999 or AOCS Cd 26-96 (03). |
Gas chromatography |
II |
E | ||
Stigmastadienes |
ISO 15788-2: 2003 |
HPLC |
CCFO is asked to consider whether the method is appropriate |
III |
TE | |
Peroxide value |
ISO 3960:2001 or AOCS Cd 8b-90 (03). |
Titrimetry |
I |
E | ||
Absorbency in ultra-violet |
COI/T.20/Doc. No. 19 or ISO 3656:2002 or AOCS Ch 5-91 (01). |
Absorption in ultra violet |
II |
E | ||
Alpha-tocopherol |
ISO 9936:1997 |
HPLC |
II |
E | ||
Olive Oils and Olive Pomace Oils |
Arsenic |
AOAC 952.13 |
Colorimetry (diethyldithiocarbamate) |
III |
E | |
Arsenic |
AOAC 942.17 |
Colorimetry (Molybdenum blue) |
III |
E | ||
Arsenic |
AOAC 986.15 |
AAS |
II |
E | ||
Lead |
AOAC 994.02 or ISO 12193:2004 or AOCS Ca 18c-91(97) |
AAS |
II |
E | ||
Traces of halogenated solvents |
COI/T.20/Doc. no. 8. |
Gas chromatography |
II |
E | ||
Moisture and volatile matter |
ISO 662:1998 |
Gravimetry |
I |
E | ||
Insoluble impurities in light petroleum |
ISO 663:2000 |
Gravimetry |
I |
E | ||
Iron and copper |
ISO 8294:1994 or AOAC 990.05 |
AAS |
II |
E | ||
Saponification value |
ISO 3657:2002 or AOCS Cd 3-25 (03) |
Titrimetry |
I |
E | ||
Unsaponifiable matter |
ISO 3596:2000 or ISO 18609:2000 or AOCS Ca 6b-53 (01) |
Gravimetry |
I |
E | ||
Fatty acids in the 2-position of the triglycerides |
ISO 6800:1997 or AOCS Ch 3-91 (02) |
Gas chromatography |
I |
E | ||
Relative density |
IUPAC 2.101, with the appropriate conversion factor |
Pycnometry |
I |
E | ||
Refractive index |
ISO 6320:2000 or AOCS Cc 7-25 (02) |
Refractometry |
II |
E | ||
Iodine value |
ISO 3961:1996 or AOAC 993.20 or AOCS Cd 1d-92 (97) or
|
Wijs-Titrimetry |
I |
E | ||
Amendments proposed to the methods in the current standard for Named Vegetable Oils
COMMODITY |
PROVISION |
METHODS |
PRINCIPLE |
TYPE |
STATUS |
Named Vegetable Oils |
Acidity |
ISO 660: 1996, amended 2003; or
|
Titrimetry |
I |
E |
Apparent density |
ISO 6883: 2000, with the appropriate conversion factor; or AOCS Cc 10c-95 (02) |
Pycnometry |
I |
E | |
Arsenic |
AOAC 952.13 |
Colorimetry (diethyldithiocarbamate) |
III |
E | |
Arsenic |
AOAC 942.17 |
Colorimetry (molybdenum blue) |
III |
E | |
Named Vegetable Oils |
Arsenic |
AOAC 986.15 |
AAS |
II |
E |
Copper and iron |
ISO 8294: 1994; or AOAC 990.05; or AOCS Ca 18b-91 (03) |
AAS |
II |
E | |
Crismer value |
AOCS Cb 4-35 (97) and AOCS Ca 5a-40 (97) |
Turbidity |
I |
E | |
GLC ranges of Fatty acid composition |
ISO 5508: 1990 and ISO 5509: 2000; or AOCS Ce 2-66 (97) and Ce 1e-91 (01) or Ce 1f-96 (02) |
Gas chromatography of methyl esters |
II |
E | |
Insoluble impurities |
ISO 663: 2000 |
Gravimetry |
I |
E | |
Iodine value (IV) |
Wijs - ISO 3961: 1996; or AOAC 993.20; or AOCS Cd 1d-1992 (97); or NMKL 39 (2003) |
Wijs-Titrimetry 2 |
I |
E | |
Lead |
AOAC 994.02 ; or ISO 12193: 2004; or
|
Atomic Absorption |
II |
E | |
Moisture & volatile matter at 105°C |
ISO 662: 1998 |
Gravimetry |
I |
E | |
Peroxide value (PV) |
AOCS Cd 8b-90 (03); or ISO 3960: 2001 |
Titrimetry |
I |
E | |
Refractive index |
ISO 6320: 2000; or AOCS Cc 7-25 (02) |
Refractometry |
II |
E | |
Reichert value and Polenske value |
AOCS Cd 5-40 (97) |
Titrimetry |
I |
E | |
Saponification value (SV) |
ISO 3657: 2002; or AOCS Cd 3-25 (03) |
Titrimetry |
I |
E | |
Slip point |
ISO 6321:2002 for all oils;
|
Open ended capillary tube |
I |
E | |
Soap content |
BS 684 Section 2.5; or AOCS Cc 17-95 (97) |
Gravimetry |
I |
E | |
Sterol content |
ISO 12228: 1999; or AOCS Ch 6-91 (97) |
Gas chromatography |
II |
E | |
Tocopherol content |
ISO 9936: 1997; or AOCS Ce 8-89 (97) |
HPLC |
II |
E | |
Unsaponifiable matter |
ISO 3596: 2000; or ISO 18609: 2000; or AOCS Ca 6b-53 (01) |
Gravimetry |
I |
E | |
B. CODEX COMMITTEE ON FISH AND FISHERY PRODUCTS3
Draft Standard for Salted Atlantic Herring and Salted Sprats (at Step 8)
Draft Amendment to the Standard for Quick Frozen Fish Sticks (Fish Fingers), Fish Portions and Fish Fillets – Breaded or in Batter
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
TYPE |
STATUS |
Salted Atlantic Herring and Salted Sprat |
Water content |
AOAC 950.46B |
air drying |
I |
E |
Quick Frozen Fish Sticks |
Fish content (declaration) |
AOAC 996.15 and calculation (see below) |
see below |
I |
E |
Section 7. Sampling, Examination and Analysis
7.4 Estimation of Fish Content
According to AOAC Method 996.15. In cases where there is some remaining doubts over the composition of the fish core then the method of analysis as outlined below could be used, i.e. as a reference method.
Determination of Fish Content
The fish content of a fish finger (fish stick) is calculated by using the following equation
For most products therefore, the fish ingredient weight is that of the raw ingredient. Any figure placed or declared on a product label would be a typical quantity reflecting the producer’s normal manufacturing variations, in accordance with good manufacturing practice.
Checking of fish content by chemical analysis
The percentage fish content, corrected for the non-fish flesh nitrogen contributed by the carbohydrate coating, is calculated as follows.
* appropriate N (nitrogen) factor
The non-fish flesh nitrogen is calculated as follows: % non-fish flesh nitrogen = % carbohydrate x 0.02
Where the carbohydrate is calculated by difference: % carbohydrate = 100 – (% water + % fat + % protein + % ash)
References
Determination of nitrogen: ISO 937:1978
Determination of moisture: ISO 1442:1997
Determination of total fat: ISO 1443:1973
Determination of ash: ISO 936: 1998
Table 2: Interim Nitrogen factors to be used for white fish as an ingredient (i.e. after GMP)
SPECIES |
Nitrogen
|
White fish: |
|
Cod |
2.66 |
Minced Cod |
2.61 |
Coley/Saithe |
2.69 |
European Hake |
2.64 |
Haddock |
2.72 |
Ling |
2.78 |
Plaice |
2.46 |
Alaskan Pollack |
2.59 |
Whiting |
2.68 |
White fish mean |
2.65 |
C. AD HOC INTERGOVERNMENTAL TASK FORCE ON FRUIT AND VEGETABLE JUICES4
1. Draft General Standard for Fruit Juices and Nectars: methods endorsed
.
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
Type |
Status |
Fruit Juices and Nectars |
Ascorbic acid-L (additives) |
IFU Method No 17a (1995) |
HPLC |
II |
E |
Ascorbic acid-L (additives) |
ISO 6557-1: 1986 |
Fluorescence spectrometry |
IV |
E | |
Ascorbic acid-L (additives) |
AOAC 967.21 |
Indophenol method |
III |
E | |
Carbon dioxide (additives and processing aids) |
IFU Method No 42 (1976) |
Titrimetry |
IV |
E | |
Cellobiose |
IFU Recommendation No.4 October 2000 |
Capillary gas chromatography |
IV |
E | |
Citric acid 5(additives) |
AOAC 986.13 |
HPLC |
II |
E | |
Citric acid 5(additives) |
EN 1137: 1994 |
Enzymatic determination |
III |
E | |
Glucose and fructose
|
EN 12630 |
HPLC |
III |
E | |
Glucose-D and fructose-D (permitted ingredients) |
EN 1140 |
Enzymatic determination |
II |
E | |
Malic acid (additives) |
AOAC 993.05 |
Enzymatic determination and HPLC |
III |
E | |
Malic acid-D |
EN 12138 |
Enzymatic determination |
II |
E | |
Malic acid-D in apple juice |
AOAC 995.06 |
HPLC |
II |
E | |
Malic acid-L |
EN 1138 (1994) |
Enzymatic determination |
II |
E | |
Pectin (additives) |
IFU Method No 26 (1964/1996) |
Precipitation/photometry |
I |
E | |
Benzoic acid and its salts; sorbic acid and its salts |
IFU Method No 63 (1995)
|
HPLC |
II |
E | |
Benzoic acid and its salts |
ISO 5518:1978
|
Spectrometry |
III |
E | |
Preservatives in fruit juices (sorbic acid and its salts) |
ISO 5519: 1978 |
Spectrometry |
III |
E | |
Saccharin |
NMKL 122 (1997) |
Liquid chromatography |
II |
E | |
Soluble solids |
AOAC 983.17 |
Indirect by refractometry |
I |
E | |
Sucrose (permitted ingredients) |
EN 12146 (1996) |
Enzymatic determination |
III |
E | |
Sucrose (permitted ingredients) |
EN 12630 |
HPLC |
II |
E | |
Sulphur dioxide (additives) |
Optimized Monier Williams AOAC 990.28
|
Titrimetry after distillation |
II |
E | |
Sulphur dioxide (additives) |
NMKL 135 (1990) |
Enzymatic determination |
III |
E | |
Sulphur dioxide (additives) |
ISO 5522:1981
|
Titrimetry after distillation |
III |
E | |
Tartaric acid in grape juice (additives) |
EN 12137 (1997) |
HPLC |
II |
E | |
Total nitrogen |
EN 12135 (1997) |
Digestion/titration |
I |
E | |
2.
Draft General Standard for Fruit Juices and Nectars: methods temporary endorsed
(subject to the finalisation by the Task Force of the provisions listed)
COMMODITY |
PROVISION |
METHOD |
PRINCPLE |
TYPE |
STATUS |
Fruit Juices and Nectars |
Acetic acid |
EN 12632 or IFU Method No 66 (1996) |
Enzymatic determination |
TE | |
Alcohol (ethanol) |
IFU Method No 52 (1983/1996) |
Enzymatic determination |
TE | ||
Anthocyanins |
IFU Method No 71 (1998) |
HPLC |
TE | ||
Ash in fruit products |
AOAC 940.26 |
Gravimetry |
TE | ||
Beet sugar in fruit juices |
AOAC 995.17 |
Deuterium NMR |
TE | ||
Benzoic acid as a marker in orange juice |
AOAC 994.11 |
HPLC |
TE | ||
Determination of C13/C12 ratio of ethanol derived from fruit juices |
JAOAC 79, No.1, 1996, 62-72 |
Stable isotope mass spectrometry |
TE | ||
Carbon stable isotope ratio of apple juice |
AOAC 981.09 - JAOAC 64, 85 (1981) |
Stable isotope mass spectrometry |
TE | ||
Carbon stable isotope ratio of orange juice |
AOAC 982.21) |
Stable isotope mass spectrometry |
TE | ||
Carotenoid, Total/individual groups |
EN 12136 (1997) - IFU Method No59 (1991) |
Precipitation/fractionation |
TE | ||
Carotenoids, Total |
ISO 6558-2:1992 |
Column chromatographic separation and spectrometry |
TE | ||
Centrifugable pulp |
EN 12134 - IFU Method No 60 (1991/1998)y |
Centrifugation/% value |
TE | ||
Chloride (expressed as sodium chloride) |
EN12133 |
Electrochemical titrimetry |
TE | ||
Chloride in vegetable juice |
AOAC 971.27 (Codex general method)
|
Titration |
TE | ||
Fruit Juices and Nectars |
Essential oils |
AOAC 968.20 - IFU 45b |
(Scott) distillation, titration |
TE | |
Essential oils (in citrus fruit) |
ISO 1955:1982 |
Distillation and direct reading of the volume |
TE | ||
Fermentability |
IFU Method No 18 (1974) |
Microbiological method |
TE | ||
Formol number |
EN 1133 (1994) |
Potentiometric titration |
TE | ||
Free amino acids |
EN 12742 |
Chromatography |
TE | ||
Fumaric acid |
IFU Method No 72 (1998) |
HPLC |
TE | ||
Glucose, fructose, sorbitol |
EN 12630 |
HPLC |
TE | ||
Gluconic acid |
IFU Method No 76 (2001) |
Enzymatic determination |
TE | ||
Glycerol |
IFU Method No 77 (2001) |
Enzymatic determination |
TE | ||
Hesperidin and naringin |
EN 12148 (1996) - IFU Method No 58 (1991) |
HPLC |
TE | ||
HFCS & HIS in apple juice (permitted ingredients) |
JAOAC 84, 486 (2001) |
CAP GC Method |
TE | ||
Hydroxymethylfurfural |
IFU Method No 69 (1996) |
HPLC |
TE | ||
Hydroxymethylfurfural |
ISO 7466:1986 |
Spectrometry |
TE | ||
Isocitric acid-D |
EN 1139 - IFU Method No 54 (1984) |
Enzymatic determination |
TE | ||
Lactic acid- D and L |
EN 12631 (1999) |
Enzymatic determination |
TE | ||
L-malic/total malic acid ratio in apple juice |
AOAC 993.05 |
TE | |||
Naringin and neohesperidin in orange juice |
AOAC 999.05 |
HPLC |
TE | ||
pH-value |
EN 1132 (1994) |
Potentiometry |
TE | ||
Phosphorus/Phosphate |
EN 1136 (1994) |
Photometric determination |
TE | ||
Proline |
EN 1141 (1994) |
Photometry |
TE | ||
Quinic acid in cranberry juice cocktail and apple juice |
AOAC 986.13 |
HPLC |
TE | ||
Recoverable oil |
AOAC 968.20 - IFU Method No 45b |
Distillation and titration Scott method |
TE | ||
Relative density |
EN 1131 (1993) |
Pycnometry |
TE | ||
Relative density |
IFU Method No 1A |
Densitometry |
TE | ||
Sodium, potassium, calcium, magnesium |
EN 1134 (1994) |
Atomic Absorption Spectroscopy |
TE | ||
Sorbitol-D |
IFU Method No 62 (1995) |
Enzymatic determination |
TE | ||
Stable carbon isotope ratio in the pulp of fruit juices |
ENV 13070 (1998) |
TE | |||
Stable carbon isotope ratio of sugars from fruit juices |
ENV 12140 |
Stable isotope mass spectrometry |
TE | ||
Stable hydrogen isotope ratio of water from fruit juices |
ENV 12142 (1997) |
Stable isotope mass spectrometry |
TE | ||
Stable oxygen isotope ratio in fruit juice water |
ENV 12141(1997) |
Stable isotope mass spectrometry |
TE | ||
Starch |
AOAC 925.38 |
Precipitation |
TE | ||
Sugar -beet derived syrups in frozen concentrated orange juice δ18O Measurements in water |
AOAC 992.09 |
Oxygen isotope ratio analysis |
TE | ||
Titrable acids, total |
EN 12147 (1995) |
Titrimetry |
TE | ||
Total dry matter |
EN 12145 (1996) |
Gravimetric determination |
TE | ||
Total solids |
AOAC 985.26 |
Microwave oven drying |
TE | ||
Vitamin C |
AOAC 967.22 |
Microfluorometry |
TE | ||
Vitamin C |
CEN/TC275/WG9 N60 |
DNA |
TE | ||
D. CODEX COMMITTEE ON NUTRITION AND FOODS FOR SPECIAL DIETARY USES
Draft Revised Standard for Gluten-Free Foods (At Step 7)
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
NOTE |
TYPE |
STATUS |
Gluten-free foods |
Gluten |
Enzyme-Linked Immunoassay R5 Mendez (ELISA) Method |
Immunoassay |
CCFNSDU to provide clarification on the application of the Method |
IV |
TE |
E. METHODS OF ANALYSIS FOR ADDITIVES AND CONTAMINANTS
1. CONTAMINANTS
Amendment to the methods endorsed by the 23rd Session of the CCMAS and adopted in 2001 (CODEX STAN 228-2001), as a result of the update of the methods for lead, copper and iron in fats and oils.
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
TYPE |
STATUS |
All foods (except fats and oils) |
Lead, cadmium, copper, iron and zinc |
NMKL 139 (1991)
|
AAS after dry ashing |
II |
E |
All foods (except fats and oils) |
Lead, cadmium, copper, iron and zinc |
NMKL 161 (1998)
|
AAS after microwave digestion |
III |
E |
Amendments to the current list of methods
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
NOTE |
TYPE |
STATUS |
All foods |
Cadmium |
AOAC 986.15 |
Anodic stripping voltametry |
III |
E | |
All foods |
Copper |
AOAC 960.40 |
Colorimetry (diethyldithiocarbamate) |
|
III |
E |
All foods |
Lead |
AOAC 972.25 |
AAS |
Type II method adopted in 2001 (see above) |
III |
E |
All foods except fats and oils |
Lead |
AOAC 982.23 |
Anodic stripping voltametry |
III |
E | |
All foods |
Lead |
AOAC 986.15 |
Anodic stripping voltametry |
III |
E | |
All foods |
Zinc |
AOAC 969.32 |
AAS |
Type II method adopted in 2001 (see above) |
III |
E |
All foods |
Zinc |
AOAC 986.15 |
AAS |
III |
E | |
|
|
|
|
Deleted as no provisions exist |
|
E |
2. ADDITIVES
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
NOTE |
TYPE |
STATUS |
Meat Products |
Nitrates and/or Nitrites |
EN 12014-3:1998-06
|
Spectrometric determination of nitrate and nitrite content of meat products after enzymatic reduction of nitrate to nitrite |
TE at the 24th session |
III6 |
E |
Meat Products |
Nitrates and/or Nitrites |
NMKL 165 (2000)
|
Ion-exchange chromatographic method |
TE at the 24th session |
III |
E |
Amendments to the current list of methods for additives
COMMODITY |
PROVISION |
METHOD |
PRINCIPLE |
NOTE |
TYPE |
STATUS |
Beverages and sweets (including fruits juices) |
Saccharin |
NMKL 122 (1997) |
Liquid chromatography |
Endorsed in 2003
|
II7 |
E |
Fats and oils |
Butylhydroxyanisole, butylhydroxytoluene, tert-butylhydroquinone, |
AOAC 983.15 |
Liquid chromatography |
nordihydroguaiaretic acid deleted as no provision exist |
II |
E |
Part II. SAMPLING
CODEX COMMITTEE ON FATS AND OILS (ALINORM 03/17, Appendix II)
Standard for Olive Oils and Olive-Pomace Oils
Sections 8.16 and Annex-Section 4.12 Sampling
According to ISO 661:1989 and ISO 5555:2001.
1 ALINORM 03/17, Appendices II, III and IV
2 It is possible to calculate the Iodine Value from fatty acid composition data obtained by gas chromatography e.g. using AOCS Cd 1b-87 (97)
3 ALINORM 04/27/18, Appendix II and Appendix VII (Draft Amendment to the Standard for Quick Frozen Fish Sticks (Fish Fingers), Fish Portions and Fish Fillets – Breaded or in Batter : declaration of fish content)
4 ALINORM 03/39A, Appendices II and III
5 All juices except citrus based juices
6 Current methods for nitrites are AOAC 973.31 as Type II and ISO 2918.1975 as Type IV (To be re-validated and updated)
7 Inclusion in the final list subject to finalization of provisions for saccharin in the Draft Standard for Fruit Juices and Nectars or in the General Standard for Food Additives