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GB 14750-2010 English PDF

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GB 14750-2010: National food safety standards -- Food additives -- Vitamin A
Status: Valid

GB 14750: Evolution and historical versions

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GB 14750-2010English229 Add to Cart 3 days [Need to translate] National food safety standards -- Food additives -- Vitamin A Valid GB 14750-2010
GB 14750-1993English239 Add to Cart 2 days [Need to translate] Food additive. Vitamin A Obsolete GB 14750-1993

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Basic data

Standard ID GB 14750-2010 (GB14750-2010)
Description (Translated English) National food safety standards -- Food additives -- Vitamin A
Sector / Industry National Standard
Classification of Chinese Standard X42
Classification of International Standard 67.220.20
Word Count Estimation 10,122
Date of Issue 2010-12-21
Date of Implementation 2011-02-21
Older Standard (superseded by this standard) GB 14750-1993
Regulation (derived from) Ministry of Health Bulletin No. 19 of 2010
Issuing agency(ies) Ministry of Health of the People's Republic of China
Summary This Chinese standard applies to the ��- ionone as starting material, obtained by chemical synthesis of food additives, vitamins A.

GB 14750-2010: National food safety standards -- Food additives -- Vitamin A

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National food safety standards - food additives - Vitamin A National Standards of People's Republic of China People's Republic of China Ministry of Health issued Issued on. 2010-12-21 2011-02-21 implementation National Food Safety Standard Vitamin A food additive

Foreword

This standard replaces GB 14750-1993 "Food Additives Vitamin A". This standard compared with GB 14750-1993, the main changes are as follows. - Vitamin A by the labeled amount "not less than 95.0%" to "97.0% -103.0%"; - Increase the TLC project identification and test methods; - Increase the lead indicators and test methods; - Increased arsenic indicators and test methods; - Increase the absorption coefficient than the target and test methods. Appendix A of this standard is a normative appendix. This standard replaces the standards previously issued as follows. --GB 14750-1993. National Food Safety Standard Vitamin A food additive

1 Scope

This standard applies to β- ionone as a starting material, obtained by chemical synthesis of food additives vitamin A.

2 Normative references

The standard file referenced in the application of this standard is essential. For dated references, only the note Version Date apply to this standard. For undated references, the latest edition (including all amendments) fitness For this standard. 3 chemical name, molecular formula, molecular mass and structural formula 3.1 Chemical Name Trans-3,7-dimethyl-9- (2,6,6-trimethyl-1-cyclohexen-1) -2,4,6,8-nonyl acetate tetraene Formula 3.2 C22H32O2 3.3 formula CH3 CH3 CH3 CH2OCOCH3 H3C CH3 3.4 relative molecular mass 328.49 (according to 2007 international relative atomic mass) 4. Technical Requirements 4.1 Sensory requirements. comply with Table 1. Table 1 Sensory requirements Project requires test methods Pale yellow color take appropriate sample is placed in a clean, dry test tube, in natural light The line, observe its color and texture, smell the smell. Odour rancid smell, almost odorless or has a slight smell of fish Tissue state in oil, frozen curable 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Vitamin A (C22H32O2) of the labeled amount a, w /% 97.0 ~ 103.0 Appendix A A.4 Acid value (in dollars KOH) (mg/g) ≤ 2.0 A.5 in Appendix A Peroxide value test by test A.6 in Appendix A The absorption coefficient ratio ≥ 0.85 A Appendix A .7 Lead (Pb)/(mg/kg) ≤ 2 GB 5009.12 Arsenic (As)/(mg/kg) ≤ 2 GB/T 5009.76 a per 1g vitamin A 10 ~ 100 million units (equivalent per 1g of vitamin A 30 mg ~ 300mg)

Appendix A

(Normative) Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive, according to the relevant provisions of the operation, I have the honor to be careful when operating Shen. If splashed on the skin should immediately wash with water, severe cases should be treated immediately. When using a volatile acid is required in the hood get on. A.2 General Provisions Unless otherwise indicated in the analysis using only recognized as analytical reagents and GB/T 6682-2008 stipulated three water. Test standard titration solution used in the method of determination of impurities standard solution, preparations and products, not specified in other When requested, according to GB/T 601, GB/T 602, the provisions of the preparation of GB/T 603's. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 chloroform. A.3.1.2 antimony trichloride solution. 250g/L chloroform solution, if necessary, use should be filtered. A.3.1.3 developing solvent. cyclohexane - ether (41). A.3.1.4 antimony trichloride test solution.200g/L chloroform solution. After use, if desired, be filtered. A.3.2 coloring test A.3.2.1 Method summary Antimony high vitamin A and an electrophilic reagent to form the unstable chlorination Jin Weng blue carbon ions. A.3.2.2 analysis step Take 1 drop of laboratory samples, add chloroform 10mL, shake to dissolve; remove the 2 drops, plus 2mL chloroform, 0.5mL Antimony trichloride solution that was blue, gradually turns purple. A.3.3 TLC A.3.3.1 Method summary Laboratory sample solution shows the same main spots of the R value of the main spots of the reference solution and the vitamin A is displayed. A.3.3.2 analysis step Weigh vitamin A reference laboratory samples and about 15000 IU placed 10mL volumetric flask, dissolved with chloroform Solution and diluted to the mark, then 0.01mL were spotted on silica gel TLC plate in developing solvent expand after started to dry. Antimony trichloride test solution color, blue spots. The main spots of the reference solution and the solution was the main spots laboratory samples displayed Consistent location. A.4 Determination of vitamin A A.4.1 Method summary Vitamin A molecule contains 5 conjugated double bonds, at a wavelength between 325nm ~ 328nm has a maximum absorption peak which most Position of the large absorption peak varies with the solvent, which can be used to determine the content. Law is at three wavelengths measured absorbance A correction value calculated based on the corrected absorbance formula, and then calculate the content. A.4.2 Reagents and materials Cyclohexane. A.4.3 Instruments and Equipment UV spectrophotometer. A.4.4 Determination A.4.4.1 analysis step Take the right amount of laboratory samples, accurate to 0.000 2 g, add cyclohexane dissolved and quantitatively diluted into 9 ~ 15 IU solution, press According vitamin A assay ( "People's Republic of China Pharmacopoeia" 2005 edition two Appendix JⅦ vitamin A assays items Dir A method) absorption peak wavelength and wavelength listed in Table A.1 absorbance was measured. Calculate the absorbance and wavelength 328nm The ratio of absorbance at a wavelength of 328nm and at a 1 mE value. Table A.1 vitamin A absorbance ratio at different wavelengths wavelength (Nm) Absorbance ratio 300 0.555 316 0.907 328 1.000 340 0.811 360 0.299 A.4.4.2 Calculation Results If the absorption peak wavelength between 326nm ~ 329nm, and the absorbance measured at each wavelength ratio does not exceed the specified A.1 ± 0.02 value using equation (A.1) content is calculated. 1 mx E = (328nm) × 1900 (A.1) Where. x-- IU of Vitamin A per gram sample contains; 1% 1cmE - percentage absorption coefficient. If the absorption peak wavelength of 326nm ~ 329nm between, but each wavelength measured absorbance ratio exceeds Table A.1 Regulation ± 0.02 of the set value, shall formula (A.2) absorbance obtained after the correction, and then calculate the content. A328 (corrected) = 3.52 (2A328-A316-A340) (A.2) Where. A328 (calibration) - absorbance at a wavelength of 328nm at after correction; A328-- absorbance at a wavelength of 328nm at; A316-- absorbance at a wavelength of 316nm at; A340-- absorbance at 340nm wavelength. If uncorrected and corrected absorbance absorbance difference does not exceed ± 3.0%, if not corrected absorbance, still uncorrected Absorbance content was calculated. If uncorrected and corrected absorbance absorbance difference between -15% to -3%, places the corrected absorbance to calculate the content. If the corrected absorbance than the uncorrected absorbance between -15% or 3%, or absorption peak wavelength of 326nm ~ not Between 329nm, the sample shall be in accordance with the "People's Republic of China Pharmacopoeia" 2005 edition two Appendix JⅦ vitamin A assay Determination under the second method (A.4.4.3). Allows parallel determination of the relative difference of less than 3%. A.4.4.3 Determination of Vitamin A second method Laboratory samples were accurately weighed amount (about the equivalent of the total amount of Vitamin A 500 IU or more, the quality of more than 2g), set soap Of the flask, add 30mL of ethanol and 3mL potassium hydroxide solution (500g/L), boiling water bath under reflux for 30min, after cooling, From top condenser water 10mL washing condenser interior wall, the saponification solution was transferred to a separatory funnel (coated piston separating funnel Starch, glycerin lubricant), 60mL ~ 100mL fractional saponification was washed with water bottles, lotion into the separating funnel, containing no Peroxides ether and shake extracted four times, each time shaking for about 5min, the first 60mL, subsequent times 40mL, combined B The ether solution was washed with water several times, each about 100mL, slowly rotating the wash should avoid emulsification, the aqueous layer until the case of phenolphthalein indicator solution Was no longer red, lined with cotton wool was washed with ether and anhydrous sodium sulfate filtered through a filter, the filter was washed with diethyl ether, wash with diethyl ether Were combined into a 250mL volumetric flask, diluted with ether, shake; precise amount of the check amount, evaporating dish inside, in The low temperature water bath evaporated to 5mL, the home vacuum dryer, drained quickly add isopropyl alcohol to dissolve and quantitative dilution made about each 1mL containing vitamin A 9 ~ 15 IU, according to the UV - visible spectrophotometry ( "People's Republic of China Pharmacopoeia" 2005 edition attached Recorded IV A), at 300nm, 310nm, 325nm and 334nm absorbance was measured at four wavelengths, and measuring the absorption peak wave long. Wavelength absorption peak should be between 323nm ~ 327nm, and the absorbance at 300nm and 325nm wavelengths at a wavelength Absorbance ratio should not exceed 0.73 calculated corrected absorbance; A325 (corrected) = 6.815A325-2.555A310-4.260A334 Laboratory vitamin A per 1g of the sample containing unit = 1 m (325nm,) 1830E × Correction If the corrected absorbance is within the uncorrected absorbance of 100% ± 3%, it is still uncorrected absorbance content was calculated. If the absorption peak wavelength of 323nm ~ 327nm is not, or between 300nm and 325nm wavelength absorbance wavelength Absorbance ratio at more than 0.73, you should extract from ether after saponification in 250mL said another precise amount of the check amount (phase When vitamin A300 ~ 400 IU), ether evaporated under reduced pressure to about left 5mL, and then in a stream of dry nitrogen, was added immediately Precision 3mL methanol, dissolved, and the precise amount of 500μL, injection of vitamin D assay ( "People's Republic of China Pharmacopoeia" 2005 Edition Appendix VII K) purification system in the second column under the law, the accurate collection of effluent containing vitamin A, in Under a stream of dry nitrogen, then in accordance with the method described above from "The rapid increase of isopropanol dissolved" since, according to the operation and calculate the content. Note 1. glycerine in the lubricant glyceryl starch 22g, soluble starch was added 9g, heated to 140 ℃, 30min stirring constantly maintained, the discharge Cold, that is, too. Note 2. The peroxide-free ether ether anesthesia according to inspection under peroxides, such as non-compliance, can be 5% sodium thiosulfate solution He was shaken, allowed to stand, the ether layer was fractionated, washed with water and shaken once distilled, end to end five percent portion was discarded, the ether distilled off further seizure Check peroxide, it should be specified. A.5 Determination of acid value A.5.1 Reagents and materials A.5.1.1 ethanol. A.5.1.2 ether. A.5.1.3 sodium hydroxide standard titration solution. c (NaOH) = 0.1mol/L. A.5.1.4 phenolphthalein indicator solution. 10g/L ethanol solution. A.5.2 Analysis step Were taken 15mL ethanol and ether, placed in a conical flask, add 5 drops of phenolphthalein indicator solution, a solution of sodium hydroxide standard titration Solution (0.1mol/L) to pale pink color, plus 2.0g laboratory samples, shaking completely dissolved with sodium hydroxide standard Titration solution (0.1mol/L) titration. A.5.3 Calculation Results Acid value (in dollars KOH) w, the value in milligrams per gram (mg/g) according to formula (A.3) Calculated. McV ×× = (A.3) Where. Numerical V-- laboratory sample consumption of sodium hydroxide standard titration solution volume in milliliters (mL); Numerical c-- actual sodium hydroxide standard titration solution concentration, expressed in moles ml (mol/L); Numerical m-- laboratory sample mass, in grams (g); M-- numerical molar mass of potassium hydroxide in grams per mole (g/mol) (M = 56.1). A.6 Determination of peroxide value A.6.1 Reagents and materials A.6.1.1 glacial acetic acid. A.6.1.2 chloroform. A.6.1.3 potassium iodide solution. take the right amount of potassium iodide to prepare a saturated solution. A.6.1.4 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1mol/L, after calibration diluted 0.01mol/L concentration Of stand-by. A.6.1.5 starch indicator solution. 5g/L. A.6.2 Analysis step Weigh about 1.0g laboratory samples, accurate to 0.000 2g. Add 30mL glacial acetic acid - chloroform (64), shaking Dissolved, add potassium iodide solution 1mL, shaking 1min, add 100mL of water and starch indicator solution 1mL sodium thiosulfate standard Titration solution (0.01mol/L) titration to the disappearance of purple blue, and titration with blank test correction, consumed thiosulfate Sodium standard titration solution (0.01mol/L) should not exceed 1.5mL. A.7 absorption coefficient ratio In the determination of items, laboratory sample solution was measured at 328nm absorbance ratio correction and direct absorption value of not less than 0.85. If the absorption peak at 326nm ~ 329nm between each and the measured absorbance ratio does not exceed a predetermined value ± 0.02, do not count Operators absorption coefficient ratio.

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