Commission Directive 2006/129/EC of 8 December 2006 amending and correcting Directive 96/77/EC laying down specific purity criteria on food additives other than colours and sweeteners (Text with EEA relevance)
1. The texts concerning E 216 propyl p-hydroxybenzoate and E 217 sodium propyl p-hydroxybenzoate are deleted. 2. The text concerning E 307 alpha-tocopherol is replaced by the following: "E 307 ALPHA-TOCOPHEROL Synonyms DL-α-Tocopherol Definition Chemical name DL-5,7,8-Trimethyltocol DL-2,5,7,8-Tetramethyl-2-(4′,8′,12′-trimethyltridecyl)-6-chromanol Einecs 233-466-0 Chemical formula C 29 H50 O2 Molecular weight 430,71 Assay Content not less than 96 % Description Slightly yellow to amber, nearly odourless, clear, viscous oil which oxidizes and darkens on exposure to air or light Identification A. Solubility tests Insoluble in water, freely soluble in ethanol, miscible in ether B. Spectrophotometry In absolute ethanol the maximum absorption is about 292 nm Purity Refractive index n D 20 1,503 to 1,507Specific absorption E 1 % 1 cm in ethanolE 1 % 1 cm (292 nm) 72 to 76(0,01 g in 200 ml of absolute ethanol) Sulphated ash Not more than 0,1 % Specific rotation [α] 25 D 0° ± 0,05° (1 in 10 solution in chloroform)Lead Not more than 2 mg/kg" 3. The text concerning E 315 erythorbic acid is replaced by the following: "E 315 ERYTHORBIC ACID Synonyms Isoascorbic acid D-Araboascorbic acid Definition Chemical name D-Erythro-hex-2-enoic acid γ-lactone Isoascorbic acid D-Isoascorbic acid Einecs 201-928-0 Chemical formula C 6 H8 O6 Molecular weight 176,13 Assay Content not less than 98 % on the anhydrous basis Description White to slightly yellow crystalline solid which darkens gradually on exposure to light Identification A. Melting range About 164 °C to 172 °C with decomposition B. Positive test for ascorbic acid/colour reaction Purity Loss on drying Not more than 0,4 % after drying under reduced pressure on silica gel for 3 hours Sulphated ash Not more than 0,3 % Specific rotation [α] 25 D 10 % (w/v) aqueous solution between – 16,5° to – 18,0°Oxalate To a solution of 1 g in 10 ml of water add 2 drops of glacial acetic acid and 5 ml of 10 % calcium acetate solution. The solution should remain clear Lead Not more than 2 mg/kg" 4. The following text concerning E 319 tertiary-butylhydroquinone (TBHQ) is inserted after E 316 sodium erythorbate: "E 319 TERTIARY-BUTYLHYDROQUINONE (TBHQ) Synonyms TBHQ Definition Chemical names Tert-butyl-1,4-benzenediol 2-(1,1-Dimethylethyl)-1,4-benzenediol Einecs 217-752-2 Chemical formula C 10 H14 O2 Molecular weight 166,22 Assay Content not less than 99 % of C 10 H14 O2 Description White crystalline solid having a characteristic odour Identification A. Solubility Practically insoluble in water; soluble in ethanol B. Melting point Not less than 126,5 °C C. Phenolics Dissolve about 5 mg of the sample in 10 ml of methanol and add 10,5 ml of dimethylamine solution (1 in 4). A red to pink colour is produced Purity Tertiary -Butyl-p -benzoquinoneNot more than 0,2 % 2,5- Di-tertiary -butyl hydroquinoneNot more than 0,2 % Hydroxyquinone Not more than 0,1 % Toluene Not more than 25 mg/kg Lead Not more than 2 mg/kg" 5. The text concerning E 415 xanthan gum is replaced by the following: "E 415 XANTHAN GUM Definition Xanthan gum is a high molecular weight polysaccharide gum produced by a pure-culture fermentation of a carbohydrate with natural strains of Xanthomonas campestris , purified by recovery with ethanol or propan-2-ol, dried and milled. It contains D-glucose and D-mannose as the dominant hexose units, along with D-glucuronic acid and pyruvic acid, and is prepared as the sodium, potassium or calcium salt. Its solutions are neutralMolecular weight Approximately 1000000 Einecs 234-394-2 Assay Yields, on dried basis, not less than 4,2 % and not more than 5 % of CO 2 corresponding to between 91 % and 108 % of xanthan gumDescription Cream-coloured powder Identification A. Solubility Soluble in water. Insoluble in ethanol Purity Loss on drying Not more than 15 % (105 °C, 2 1 /2 hours)Total ash Not more than 16 % on the anhydrous basis determined at 650 °C after drying at 105 °C for four hours Pyruvic acid Not less than 1,5 % Nitrogen Not more than 1,5 % Ethanol and propan-2-ol Not more than 500 mg/kg singly or in combination Lead Not more than 2 mg/kg Total plate count Not more than 5000 colonies per gramYeast and mould Not more than 300 colonies per gram E. coli Absent in 5 g Salmonella spp.Absent in 10 g Xanthomonas campestris Viable cells absent in 1 g" 6. The following text concerning E 426 soybean hemicellulose is inserted after E 425(ii) konjac glucomannan: "E 426 SOYBEAN HEMICELLULOSE Synonyms Definition Soybean hemicellulose is a refined water-soluble polysaccharide obtained from natural strain soybean fibre by hot water extraction Chemical names Water soluble soybean polysaccharides Water soluble soybean fibre Assay Not less than 74 % carbohydrate Description Free flowing spray-dried white powder Identification A. Solubility Soluble in hot and cold water without gel formation pH of 1 % solution 5,5 ± 1,5 B. Viscosity of 10 % solution Not more than 200 mPa.s Purity Loss on drying Not more than 7 % (105 °C, 4 h) Protein Not more than 14 % Total ash Not more than 9,5 % (600 °C, 4 h) Arsenic Not more than 2 mg/kg Lead Not more than 5 mg/kg Mercury Not more than 1 mg/kg Cadmium Not more than 1 mg/kg Standard plate count Not more than 3000 colonies per gramYeast and mould Not more than 100 colonies per gram E. Coli Negative in 10 g" 7. The following text concerning E 462 ethyl cellulose is inserted after E 461 methyl cellulose: "E 462 ETHYL CELLULOSE Synonyms Cellulose ethyl ether Definition Ethyl cellulose is cellulose obtained directly from fibrous plant material and partially etherified with ethyl groups Chemical names Ethyl ether of cellulose Chemical formula The polymers contain substituted anhydroglucose units with the following general formula: C 6 H7 O2 (OR1 )(OR2 ) where R1 and R2 may be any of the following:H CH 2 CH3
Assay Content not less than 44 % and not more than 50 % of ethoxyl groups (-OC 2 H5 ) on the dried basis (equivalent to not more than 2,6 ethoxyl groups per anhydroglucose unit)Description Slightly hygroscopic, white to off white, odourless and tasteless powder Identification A. Solubility Practically insoluble in water, in glycerol and in propane-1,2-diol but soluble in varying proportions in certain organic solvents depending upon the ethoxyl content. Ethyl cellulose containing less than 46 to 48 % of ethoxyl groups is freely soluble in tetrahydrofuran, in methyl acetate, in chloroform and in aromatic hydrocarbon ethanol mixtures. Ethyl cellulose containing 46 to 48 % or more of ethoxyl groups is freely soluble in ethanol, in methanol, in toluene, in chloroform and in ethyl acetate B. Film forming test Dissolve 5 g of the sample in 95 g of an 80:20 (w/w) mixture of toluene ethanol. A clear, stable, slightly yellow solution is formed. Pour a few ml of the solution onto a glass plate and allow the solvent to evaporate. A thick, tough, continuous, clear film remains. The film is flammable Purity Loss on drying Not more than 3 % (105 °C, 2 h) Sulphated ash Not more than 0,4 % pH of a 1 % colloidal solution Neutral to litmus Arsenic Not more than 3 mg/kg Lead Not more than 2 mg/kg Mercury Not more than 1 mg/kg Cadmium Not more than 1 mg/kg" 8. The text concerning E 472c citric acid esters of mono- and diglycerides of fatty acids is replaced by the following: "E 472c CITRIC ACID ESTERS OF MONO- AND DIGLYCYERIDES OF FATTY ACIDS Synonyms Citrem Citric acid esters of mono- and diglycerides Citroglycerides Mono- and diglycerides of fatty acids esterified with citric acid Definition Esters of glycerol with citric acid and fatty acids occurring in food oils and fats. They may contain small amounts of free glycerol, free fatty acids, free citric acid and free glycerides. They may be partially or wholly neutralised with sodium hydroxide or with potassium hydroxide Description Yellowish or light brown liquids to waxy solids or semi-solids Identification A. Positive test for glycerol, for fatty acids and for citric acid B. Solubility Insoluble in cold water Dispersible in hot water Soluble in oils and fats In soluble in cold ethanol Purity Acids other than citric and fatty acids Not detectable Free glycerol Not more than 2 % Total glycerol Not less than 8 % and not more than 33 % Total citric acid Not less than 13 % and not more than 50 % Sulphated ash (determined at 800 ± 25 °C) Non-neutralised products: not more than 0,5 % Partially or wholly neutralised products: not more than 10 % Lead Not more than 2 mg/kg Free fatty acids Not more than 3 % estimated as oleic acid Purity criteria apply to the additive free of sodium, potassium and calcium salts of fatty acids, however, these substances may be present up to a maximum level of 6 % (expressed as sodium oleate). "9. The text concerning E 559 aluminium silicate (kaolin) is replaced by the following: "E 559 ALUMINIUM SILICATE (KAOLIN) Synonyms Kaolin, light or heavy Definition Aluminium silicate hydrous (kaolin) is a purified white plastic clay composed of kaolinite, potassium aluminium silicate, feldspar and quartz. Processing should not include calcination. The raw kaolinitic clay used in the production of aluminium silicate shall have a level of dioxin which does not make it injurious to health or unfit for human consumption Einecs 215-286-4 (kaolinite) Chemical formula Al 2 Si2 O5 (OH)4 (kaolinite)Molecular weight 264 Assay Content not less than 90 % (sum of silica and alumina, after ignition) Silica (SiO 2 ) Between 45 % and 55 %Alumina (A1 2 O3 ) Between 30 % and 39 %Description Fine, white or greyish white, unctuous powder. Kaolin is made up of loose aggregations of randomly oriented stacks of kaolinite flakes or of individual hexagonal flakes. Identification A. Positive test for alumina and for silicate B. X-ray diffraction Characteristic peaks at 7,18/3,58/2,38/1,78 Å C. IR absorption Peaks at 3700 and3620 cm–1 Purity Loss on ignition Between 10 and 14 % ( 1000 °C, constant weight)Water soluble matter Not more than 0,3 % Acid soluble matter Not more than 2 % Iron Not more than 5 % Potassium oxide (K 2 O)Not more than 5 % Carbon Not more than 0,5 % Arsenic Not more than 3 mg/kg Lead Not more than 5 mg/kg Mercury Not more than 1 mg/kg" 10. The following text concerning E 586 4-hexylresorcinol is inserted after E 578 calcium gluconate: "E 586 4-HEXYLRESORCINOL Synonyms 4-Hexyl-1,3-benzenediol Hexylresorcinol Definition Chemical names 4-Hexylresorcinol Einecs 205-257-4 Chemical formula C 12 H18 O2 Molecular weight 197,24 Assay Not less than 98,0 % on the dried basis Description White powder Identification A. Solubility Freely soluble in ether and acetone; very slightly soluble in water B. Nitric acid test To 1 ml of a saturated solution of the sample, add 1 ml of nitric acid. A light red colour appears C. Bromine test To 1 ml of saturated solution of the sample, add 1 ml of bromine TS. A yellow, flocculent precipitate dissolves producing a yellow solution D. Melting range 62 to 67 °C Purity Acidity Not more than 0,05 % Sulphated ash Not more than 0,1 % Resorcinol and other phenols Shake about 1 g of the sample with 50 ml of water for a few minutes, filter, and to the filtrate add 3 drops of ferric chloride TS. No red or blue colour is produced Nickel Not more than 2 mg/kg Lead Not more than 2 mg/kg Mercury Not more than 3 mg/kg" 11. The following text concerning E 1204 pullulan is inserted after E 1200 polydextrose: "E 1204 PULLULAN Definition Linear, neutral glucan consisting mainly of maltotriose units connected by -1,6 glycosidic bonds. It is produced by fermentation from a food grade hydrolysed starch using a non-toxin producing strain of Aureobasidium pullulans . After completion of the fermentation, the fungal cells are removed by microfiltration, the filtrate is heat-sterilised and pigments and other impurities are removed by adsorption and ion exchange chromatographyEinecs 232-945-1 Chemical formula (C 6 H10 O5 )x Assay Not less than 90 % of glucan on the dried basis Description White to off-white odourless powder Identification A. Solubility Soluble in water, practically insoluble in ethanol. B. pH of 10 % solution 5,0 to 7,0 C. Precipitation with polyethylene glycol 600 Add 2 ml of polyethylene glycol 600 to 10 ml of a 2 % aqueous solution of pullulan. A white precipitate is formed D. Depolymerisation with pullulanase Prepare two test tubes each with 10 ml of a 10 % pullulan solution. Add 0,1 ml pullulanase solution having activity 10 units/g to one test tube, and 0,1 ml water to the other. After incubation at about 25 °C for 20 min, the viscosity of the pullulanase-treated solution is visibly lower than that of the untreated solution Purity Loss on drying Not more than 6 % (90 °C, pressure not more than 50 mm Hg, 6 h) Mono-, di- and oligosaccharides Not more than 10 % expressed as glucose Viscosity 100 to 180 mm 2 /s (10 % w/w aqueous solution at 30 °C)Lead Not more than 1 mg/kg Yeast and moulds Not more than 100 colonies per gram Coliforms Absent in 25 g Salmonella Absent in 25 g" 12. The following text concerning E 1452 starch aluminium octenyl succinate is inserted after E 1451 acetylated oxidised starch: "E 1452 STARCH ALUMINIUM OCTENYL SUCCINATE Synonyms SAOS Definition Starch aluminium octenyl succinate is starch esterified with octenylsuccinic anhydride and treated with aluminium sulphate Description White or nearly white powder or granules or (if pregelatinised) flakes, amorphous powder or coarse particles Identification A. If not pregelatinised: by miscroscopic observation B. Iodine staining positive (dark blue to light red colour) Purity (all values expressed on an anhydrous basis except for loss on drying) Loss on drying Not more than 21 % Octenylsuccinyl groups Not more than 3 % Octenylsuccinic acid residue Not more than 0,3 % Sulphur dioxide Not more than 50 mg/kg for modified cereal starches Not more than 10 mg/kg for the other modified starches unless otherwise specified Arsenic Not more than 1 mg/kg Lead Not more than 2 mg/kg Mercury Not more than 0,1 mg/kg Aluminium Not more than 0,3 %"