REVIEW AND UPDATE OF METHODS IN CXS 234 Recommended methods of analysis for milk and milk products

Transcription

1 Agenda tem 4 JONT FAO/WHO FOOD STANDARDS PROGRAMME CODEX COMMTTEE ON METHODS OF ANALYSS AND SAMPLNG 39 th Session Budapest, Hungary, 7-11May 2018 CX/MAS 18/39/4 Add.1 March 2018 REVEW AND UPDATE OF METHODS N CXS 234 Recommended methods of analysis for milk and milk products (Prepared by AOAC/DF/SO) NTRODUCTON At its38 th session, CCMAS agreed to continue efforts on the workable packages for the review and update of CODEX STAN (CXS ) as described in CX/MAS 17/38/6. The Committee also agreed to pilot this effort through an update of all methods related to milk and milk products with the assistance of DF, SO and AOAC (REP 17/MAS, 58-59). AOAC, DF and SO welcome the opportunity to present to CCMAS their review of the dairy products package. AOAC/DF/SO have reviewed all methods relating to milk and milk products, and have identified some issues that require attention by the Committee (see Recommendations and Table below). For commodities/provisions in the Table with no comments, AOAC/DF/SO confirm that the current information is correct. RECOMMENDATONS n the preamble of CXS 234 or other suitable place, CCMAS to Clarify rules for determining when a defining method should be Type or Type V method. For example: o o s it necessary to have precision figures for a Type method? f a defining method has been subjected to an international collaborative study involving dairy commodities A, B and C, and the method is generally known to work on commodity D, but this commodity was not included in the study, should the method then be listed as Type or Type V in CXS 234 for commodity D? Clarify for the situation where there are two defining methods (from different organisations) and the degree of validation differs (i.e. one method has been subjected to an international collaborative study, whereas the other method has not), whether one method be Type and the other method Type V, or only one (the best validated) method should be accepted and be listed as Type. Clarify for those cases where a provision is not specifically listed in the Commodity Standard, what decision process is to be followed to determine whether or not to include such provision in CXS 234 (e.g., see provisions for iron in milk products, lead in edible casein products, and MSNF in cream in the table below). Apply a consistent approach in listing provisions that require a calculation based on two or more analyses. n some cases, all concerned methods are listed; in other cases only a single method (see example of inconsistency below).

2 CX/MAS 18/39/4 Add.1 Cottage cheese Fat-free dry matter SO 5534 DF 4 and SO 1735 DF 5 Cheeses in brine Milk fat in dry matter (FDM) SO 1735 DF 5 Calculation from dry matter content and fat content Gravimetry, drying at 102 C Gravimetry (Schmid-Bondzynski- Ratzlaff) Gravimetry (Schmid-Bondzynski- Ratzlaff)

3 CX/MAS 18/39/4 Add.1 3 Milk products ron NMKL139AOAC Atomic absorption spectrophotometry (Codex general method) Comment: There is no standard for milk products and no provision for iron in nutrition labelling nor GSTCFF. There are provisions for iron in butter, milk fat products, whey powders and edible casein products. AOAC as written has only been validated in milk powder, does not contain precision data or specify applicability to milk products. A separator is needed between NMKL 139 AOAC 999.1, forward slash or vertical line as appropriate. Milk products ron NMKL161/ Atomic absorption spectrophotometry AOAC Comment: There is no standard for milk products and no provision for iron in nutrition labelling nor GSTCFF. There are provisions for iron in butter, milk fat products, whey powders and edible casein products. AOAC as written is not applicable to foods 40%fat, specifically states not applicable to milk powder, does not contain precision data or specify applicability to milk products. Milk products ron AOAC nductively Coupled Plasma optical emission spectrophotometry Comment: There is no standard for milk products and no provision for iron in nutrition labelling nor GSTCFF. There are provisions for iron in butter, milk fat products, whey powders and edible casein products. AOAC as written has only been validated in infant formula and does not include precision data or specify applicability to milk products. Milk products ron SO6732 DF103 Photometry (bathophenanthroline) V Comment: There is no standard for milk products and no provision for iron in nutrition labelling nor GSTCFF. There are provisions for iron in butter, milk fat products, whey powders and edible casein products. Melamine SO/TS15495 DF/RM230 LC-MS/MS V Comment: There is no standard for milk products.

4 CX/MAS 18/39/4 Add.1 4 Milk products (products not completely Milk fat SO DF124-3 Gravimetry (Weibull-Berntrop) soluble in ammonia) Comment: There is no standard for milk products. Blend of evaporated skimmed milk and vegetable fat Blend of evaporated skimmed milk and vegetable fat Blend of evaporated skimmed milk and vegetable fat Blend of evaporated skimmed milk and vegetable fat Reduced fat blend of evaporated skimmed milk and vegetable fat Reduced fat blend of evaporated skimmed milk and vegetable fat Comment: Note 15 is needed Reduced fat blend of evaporated skimmed milk and vegetable fat Reduced fat blend of evaporated skimmed milk and vegetable fat Blend of skimmed milk and vegetable fat in powdered form Blend of skimmed milk and vegetable fat in powdered form Blend of skimmed milk and vegetable fat in powdered form Blend of skimmed milk and vegetable fat in powdered form Total fat SO1737 DF13 Gravimetry (Röse-Gottlieb) Milk solids-notfat SO6731 DF21andSO1737 D Calculation from total solids content and fat content 15 (MSNF) F13 Gravimetry (Röse-Gottlieb) Milk protein in MSNF 15 SO DF20-1 Titrimetry (Kjeldahl) V Milk protein in MSNF 15 AOAC991./20 Titrimetry (Kjeldahl) V Total fat SO1737 DF13 Gravimetry (Röse-Gottlieb) Milksolids-not-fat 15 (MSNF) SO6731 DF21 andso1737 DF13 Calculation from total solids content and fat content Gravimetry (Röse-Gottlieb) MilkproteininMSNF 15 SO DF20-1/ Titrimetry (Kjeldahl) V MilkproteininMSNF 15 AOAC Titrimetry (Kjeldahl) V Total fat SO1736 DF9 Gravimetry (Röse-Gottlieb) Water 16 SO5537 DF26 Gravimetry,dryingat87 C MilkproteininMSNF 15 SO DF20-1/ Titrimetry (Kjeldahl) V MilkproteininMSNF 15 AOAC Titrimetry (Kjeldahl) V 15 Milk total solids and Milk solids-not-fat (MSNF) content include water of crystallization of lactose 16 Water content excluding the crystallized water bound to lactose (generally known as moisture content )

5 CX/MAS 18/39/4 Add.1 5 Comment: The content of the line was missing Reduced fat blend of skimmed milk powder and vegetable fat in powdered form Reduced fat blend of skimmed milk powder and vegetable fat in powdered form Reduced fat blend of skimmed milk powder and vegetable fat in powdered form Reduced fat blend of skimmed milk powder and vegetable fat in powdered form Blend of sweetened condensed skimmed milk and vegetable fat Blend of sweetened condensed skimmed milk and vegetable fat Blend of sweetened condensed skimmed milk and vegetable fat Comment: note 15 needed. Reduced fat blend of sweetened condensed skimmed milk and vegetable fat Reduced fat blend of sweetened condensed skimmed milk and vegetable fat Reduced fat blend of sweetened condensed skimmed milk and vegetable fat Reduced fat blend of sweetened condensed skimmed milk and vegetable fat t Total fat SO1736 DF9 Gravimetry (Röse-Gottlieb) Water 16 SO5537 DF26 Gravimetry, drying at87 C Milk protein in MSNF 15 SO DF20-1 Titrimetry (Kjeldahl) V Milk protein in MSNF 15 AOAC Titrimetry (Kjeldahl) V Total fat SO1737 DF13 Gravimetry (Röse-Gottlieb) Sucrose SO2911 DF35 Polarimetry V Milksolids-not-fat 15 (MSNF) SO6734 DF15 Calculation from total solids content, fat content and sugar content Milk protein in MSNF 15 SO DF20-1 Titrimetry (Kjeldahl) V Milk protein in MSNF 15 AOAC Titrimetry (Kjeldahl) V Total fat SO1737 DF13 Gravimetry (Röse-Gottlieb) Milksolids-not-fat 15 (MSNF) SO6734 DF15 Calculation from total solids content and sugar content V V

6 CX/MAS 18/39/4 Add.1 6 Comment: note 15 needed. Reduced fat blend of sweetened MilkproteininMSNF 15 SO DF20-1 Titrimetry (Kjeldahl) V condensed skimmed milk and vegetable fat Reduced fat blend of sweetened MilkproteininMSNF 15 AOAC Titrimetry (Kjeldahl) V condensed skimmed milk and vegetable fat Butter Copper SO5738 DF76 AOAC Photometry, diethyldithiocarbamate Comment: The DF/SO method and AOAC method are different and should be written in different lines. AOAC as written does not contain precision data or specify applicability to butter. Butter Lead AOAC972.25(Codex general method) Atomic absorption spectrophotometry Comment: AOAC as written does not contain precision data or specify applicability to butter. Butter Milksolids-not-fat 15 (MSNF) SO DF80-2 Gravimetry Comment: note 15 needed. Butter Milkfat SO17189 DF194 Gravimetry Direct determination of fat using solvent extraction Butter Milkfat purity SO17678 DF202 Calculation from determination of triglycerides by gas chromatography Butter Salt SO1738 DF12/AOAC Titrimetry(Mohr:determinationofchloride,expressedassodi umchloride) Butter Salt SO15648 DF179 Potentiometry (determination of chloride, expressed as sodium chloride) Butter Vegetable fat SO12078 DF159 Gaschromatography (sterols) Butter Vegetable fat (sterols) SO18252 DF200 Gaschromatography Butter Water 16 SO DF80-1 Gravimetry

7 CX/MAS 18/39/4 Add.1 7 Comment: Correct references are SO DF 80-1 Cheese Citric acid SO/TS2963 DF/RM34 Enzymatic method V Cheese Citric acid AOAC Photometry Comment: AOAC as written does not include precision data. Cheese Milkfat SO1735 DF5 Gravimetry (Schmid-Bondzynski-Ratslaff) Cheese Moisture SO5534 DF4 Gravimetry,dryingat102 C Cheese (and cheese rind) Natamycin SO DF140-1 Molecular absorption spectrophotometry Comment: Shall the two lines above be fully separated as the two methods have different types? SO DF140-2 HPLC Cheese Sodium chloride SO5943 DF88 Potentiometry (determination of chloride, expressed as sodium chloride) Cheeses, individual Dry matter(total solids) SO5534 DF4 Gravimetry,dryingat102 C Cheeses, individual Milkfat in dry matter SO1735 DF5 Gravimetry (Schmid-Bondzynski-Ratzlaff) Cheeses, individual Dry matter(total solids) 15 SO5534 DF4 Gravimetry,dryingat102 C Comment: The two lines above may need to be combined, as both SO 1735 DF5 and SO 5534 DF 4 are needed to determine milkfat in dry matter (see fat-free dry matter for cottage cheese for instance). CCMAS to clarify a consistent format when combination of several methods. Cheeses in brine Milkfat in dry matter SO1735 DF5 Gravimetry (Schmid-Bondzynski-Ratzlaff) (FDM) Cottage cheese Fat-free dry matter SO5534 DF4and Calculation from dry matter content and fat content SO1735 DF5 Gravimetry,dryingat102 CGravimetry(Schmid- Bondzynski-Ratzlaff) Cottage cheese Milkfat SO1735 DF5 Gravimetry (Schmid-Bondzynski-Ratzlaff) (for samples containing lactose up to 5%)

8 CX/MAS 18/39/4 Add.1 8 SO DF124-3 Gravimetry (Weibull-Berntrop) (for samples containing lactose over 5%) Cottage cheese Milkfat in dry matter SO DF124-3 Gravimetry (Weibull-Berntrop) Comment: SO5534 DF4 must be added for dry matter determination. Also, SO 1735 DF 5 is preferable to SO DF SO 1735 DF 5 is fully applicable to cottage cheese unless the cheese contains non-dairy ingredients like sugar, jam, muesli. For these added products SO DF is more appropriate. Cheese, Unripened ncluding Fresh Milk Protein SO DF20-1 Titrimetry, Kjeldahl Cheese Cream and Prepared Creams Milk protein SO DF20-1 Titrimetry (Kjeldahl) Cream Milkfat SO2450 DF16 Gravimetry (Röse-Gottlieb) Cream Solids 15 SO6731 DF21 Gravimetry (drying at 102 C) Comment: note 15 needed. Creams Lowered in Milkfat Content Milkfat SO2450 DF16/AOAC Gravimetry(Röse-Gottlieb) Creams, Whipped Creams and Fermented Creams Milksolids-not-fat (MSNF) 15 SO DF80-2 AOAC Gravimetry Comment: There appears to be no requirement for MSNF in CXS 288 for creams and prepared creams, therefore CCMAS to confirm the need for this provision in CXS 234. AOAC is not equivalent to the SO DF method, therefore the method should be listed in separate lines Neither the SO DF method nor the AOAC method have been validated for this commodity. Cream cheese Dry matter SO5534 DF4 Gravimetry drying at102 C (forced air oven) Cream cheese Moisture on fat free basis SO5534 DF4 SO1735 DF5 Calculation from fat content and moisture content Gravimetry drying at102 C(forced air oven) Gravimetry (Schmid-Bondzynski-Ratzlaff) Dairy fat spreads Milkfat purity SO17678 DF202 Calculation from determination of triglycerides by gas chromatography Dairy fat spreads Total fat SO17189 DF194 Gravimetry Direct determination of fat using solvent extraction

9 CX/MAS 18/39/4 Add.1 9 Dairy fat spreads Vegetable fat (sterols) SO12078 DF159 Gas chromatography Dairy fat spreads Vegetable fat (sterols) SO18252 DF200 Gas chromatography Edible casein products Acids, free SO5547 DF91 Titrimetry (aqueous extract) V Edible casein products Ash(includingP2O5) SO5545 DF90 Gravimetry (ashingat825 C) or 17 SO5544 DF89 Edible casein products Copper AOAC Atomic absorption spectrophotometry Edible casein products Copper SO5738 DF76 Colorimetry(diethyldiethiocarbamate) Edible casein products Lactose SO5548 DF106 Photometry(phenol and H2SO4) V Edible casein products Lead NMKL139 (Codex general method) AOAC Atomic absorption spectrophotometry Comment: There is no provision for lead in CXS 290 for edible casein products. AOAC as written has only been validated in milk powder and does not contain precision data or specify applicability to edible casein products. Edible casein products Lead NMKL161/AOAC Atomic absorption spectrophotometry Comment: There is no provision for lead in CXS 290 for edible casein products. AOAC as written does not contain precision data or specify applicability to edible casein products. Edible casein products Lead AOAC972.25(Codex general method) Atomic absorption spectrophotometry Comment: There is no provision for lead in CXS 290 for edible casein products. AOAC as written does not contain precision data or specify applicability to edible casein products. Edible casein products Lead AOAC982.23(Codex general method) Anodic stripping voltanmetry Comment: There is no provision for lead in CXS 290 for edible casein products. AOAC as written does not contain precision data or specify applicability to edible casein products. 17 Refer to scope of the methods

10 CX/MAS 18/39/4 Add.1 10 Edible casein products Lead SO/TS6733 DF/RM133 Spectrophotometry(1,5-diphenylthiocarbazone) V Comment: There is no provision for lead in CXS 290 for edible casein products. Edible casein products Milkfat SO5543 DF127 Gravimetry (Schmid-Bondzynski-Ratslaff) Edible casein products ph SO5546 DF115 Electrometry V Edible casein products Milk SO DF20-1 Titrimetry, Kjeldahl Protein(totalNx6.38indrym atter) Edible casein products Sediment(scorched SO5739 DF107 Visual comparison with standard disks, after filtration V particles) Edible casein products Water 16 SO5550 DF78 Gravimetry (dryingat102 C) Emmental Calcium SO8070 DF119 Flame atomic absorption V >=800mg/100g Evaporated milks Milkfat SO1737 DF13 Gravimetry (Röse-Gottlieb) Evaporated milks Milk Protein in MSNF 15 SO DF20-1 Titrimetry (Kjeldahl) Evaporated milks Solids, total 15 SO6731 DF21 Gravimetry (drying at 102 C) Fermented milks Colony-forming units of SO6611 DF94 Colony-count at 25 C V yeasts and/or moulds Fermented milks Dry matter (total solids) 15 SO13580 DF151 Gravimetry (drying at102 C) Comment: note 15 needed. Fermented milks Ttotal acidity expressed as percentage of lactic acid SO/TS11869 DF/RM150 Potentiometry,titrationtopH8.30 Fermented milks Lactobacillus acidophilus SO20128 DF192 Colonycountat37 C

11 CX/MAS 18/39/4 Add.1 11 Fermented milks - Yoghurt and yoghurt products Fermented milks - Yoghurt and yoghurt products Fermented milks Lactobacillus delbrueckii subsp bulgaricus & Streptococcus thermophilus Lactobacillus delbrueckii subsp bulgaricus & Streptococcus thermophilus Microorganisms constituting the starter culture SO7889 DF117 Colony count at37 C SO9232 DF146 Test for strain identification SO27205 DF149 (Annex A) Colony count at 25 C, 30 C, 37 C and 45 C according to the starter organism in question Fermented milks Milkfat SO1211 DF1/AOAC Gravimetry (Röse-Gottlieb) Comment: The DF/SO and AOAC methods are different and neither have been specifically validated for fermented milks. Fermented milks Milk Protein SO DF20-1 Titrimetry( Kjeldahl) Milk powders and cream powders Acidity, titratable SO6091 DF86 Titrimetry,titrationtopH8.4 Milk powders and cream powders Milkfat SO1736 DF9 Gravimetry (Röse-Gottlieb) Milk powders and cream powders Milk Protein SO DF20-1 Titrimetry (Kjeldahl) Milk powders and cream powders Scorched particles SO5739 DF107 Visual comparison with standard disks, after filtration V Solubility ndex SO8156 DF129 Centrifugation Milk powders and cream powders Water 16 SO5537 DF26 18 Gravimetry (drying at 87 C) V Milkfat products Copper SO5738 DF76 AOAC Photometry, diethyldithiocarbamate Comment: AOAC as written does not contain precision data or specify applicability to milk fat products. The DF/SO method and AOAC method are different and should be written in different lines. Milkfat products Fatty acids, free (expressed as oleic acid) SO1740 DF6 Titrimetry

12 CX/MAS 18/39/4 Add.1 12 Milkfat products Milkfat purity SO17678 DF202 Calculation from determination of triglycerides by gas chromatography Milkfat products (anhydrous milkfat) Peroxide value (expressed SO3976 DF74 Photometry as meq. of oxygen/kg fat) Comment: Clarification to match provision in CXS 280 for Milkfat Products. Milkfat products (anhydrous milkfat) Peroxide value AOAC Titrimetry Comment: AOAC as written does not contain precision data. Milkfat products Vegetable fat(sterols) SO12078 DF159 Gas chromatography SO18252 DF200 Gas chromatography Comment: Shall the two lines above be fully separated as the two methods have different types? Milk fat products Water SO5536 DF23 Titrimetry (KarlFischer) Milk fat products (anhydrous milk fat) Peroxide value SO3976 DF74 Photometry Milk fat products (anhydrous milkfat) Peroxide value AOAC Titrimetry Comment: Duplicates of lines above. Mozzarella Milk fat in dry matter with high moisture SO1735 DF5 Gravimetry after solvent extraction Mozzarella Milk fat in dry matter with SO1735 DF5 Gravimetry after solvent extraction low moisture Sweetened Condensed Milks Milkfat SO1737 DF13 Gravimetry (Röse-Gottlieb) Sweetened Condensed Milks MilkProteininMNSF 15 SO DF20-1 Titrimetry (Kjeldahl) Sweetened Condensed Milks Solids 15 SO6734 DF15 Gravimetry,dryingat102 C Comment: note 15 needed

13 CX/MAS 18/39/4 Add.1 13 Whey cheeses by coagulation Milkfat SO1735 DF5 Gravimetry (Schmid-Bondzynski-Ratzlaff) Whey cheeses by coagulation Milk fat in dry matter SO1735 DF5 andso5534 DF4 Calculation from fat content and dry matter content Gravimetry (Schmid-Bondzynski- RatzlaffGravimetry,dryingat102 C Whey cheeses by concentration Milkfat SO1854 DF59 Gravimetry (Röse-Gottlieb) Whey cheeses by concentration Milk fa in dry matter SO1854 DF59andSO2920 D Calculation from fat content and dry matter content F58 Gravimetry (Röse-Gottlieb) Gravimetry, drying at 88 C Whey powders Ash SO5545 DF90 Gravimetry (ashingat825 C) V Whey powders Copper AOAC Atomic absorption spectrophotometry Whey powders Copper SO5738 DF76 Photometry(diethyldithiocarbamate) Whey powders Lactose SO5765-1/2 DF79-1/2 Enzymaticmethod:Part1-GlucosemoietyorPart2- Galactosemoiety Whey powders Lead AOAC (Codex general Atomic absorption spectrophotometry method) Comment: AOAC as written does not contain precision data or specify applicability to whey powders. Whey powders Milkfat SO1736 DF 9 Gravimetry (Röse-Gottlieb) Whey powders Milk protein(totalnx6.38) SO DF20-1 Titrimetry (Kjeldahl) Whey powders Moisture, "Free" SO2920 DF58 Gravimetry (drying at 88 C ±2 C) V Whey powders Water 16 SO5537 DF26 Gravimetry (drying at 87 C)

14 CX/MAS 18/39/4 Add.1 14 Proposed new methods Cheese Propionic acid SO/TS DF/RM Gas chromatography V Cheese Propionic acid SO/TS DF/RM on exchange chromatography V Comment: CXS 283 General Standard for Cheese has a maximum level of 3000 mg/kg for propionic acid.