GB 14755-2010 English PDF

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GB 14755-2010: National food safety standards -- Food additives -- Vitamin D2 (lysergic ergocalciferol)
Status: Valid

GB 14755: Historical versions

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 14755-2010	299	Add to Cart	3 days	National food safety standards -- Food additives -- Vitamin D2 (lysergic ergocalciferol)	Valid
GB 14755-1993	239	Add to Cart	2 days	Food additive. Vitamin D2 (Ergocalciferol)	Obsolete

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Basic data

Standard ID: GB 14755-2010 (GB14755-2010)
Description (Translated English): National food safety standards -- Food additives -- Vitamin D2 (lysergic ergocalciferol)
Sector / Industry: National Standard
Classification of Chinese Standard: C54;X40
Classification of International Standard: 67.220.20
Word Count Estimation: 13,172
Date of Issue: 2010-12-21
Date of Implementation: 2011-02-21
Older Standard (superseded by this standard): GB/T 14755-1993
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 ergosterol for raw materials for food additives vitamin D2.

GB 14755-2010: National food safety standards -- Food additives -- Vitamin D2 (lysergic ergocalciferol)

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
National food safety standards - food additives - vitamin D2 (lysergic ergocalciferol) 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 Food additive vitamin D2 (ergocalciferol)

Foreword

This standard replaces GB 14755-1993 "Food additive vitamin D2". This standard compared with GB 14755-1993, the main changes are as follows. - Added Infrared Spectroscopy; - Determination of vitamin D2 system suitability test of the sample to the vitamin D2 vitamin D3, the content was measured by HPLC The method of the internal standard method to the external standard method; - Digitonin test checks ergosterol amended as thin layer chromatography; - An increase of reducing substance indicators and test methods; - An increase of heavy metal indicator and test methods; - Increased arsenic indicators and test methods. The Standard Annexes A and B are normative appendix Appendix C is informative appendix. This standard replaces the standards previously issued as follows. --GB 14755-1993 National Food Safety Standard Food additive vitamin D2 (ergocalciferol)

1 Scope

This standard applies to ergosterol for raw materials of food additive vitamin D2.

2 Normative references

The standard file referenced in the application of this standard is essential. For cited documents with dates, only the date of Version applies to this standard. For undated references, the latest edition (including any amendments) applies to this standard. 3 chemical name, molecular formula, molecular mass and structural formula 3.1 Chemical Name 9,10 open loop ergot 5,7,10 (19), 22-tetraene--3β- alcohol Formula 3.2 C28H44O 3.3 formula CH2 HO CHCH H3C CH3 CHCH CH3 CH (CH3) 2 3.4 relative molecular mass 396.66 (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 Colorless or white color proper amount of sample is placed in a clean, dry test tube, in natural light The line, observe the color and texture, smell the smell. Odour odorless Organization Status needle crystal or crystalline powder 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Vitamin D2 (C28H44O), /% 98.0 ~ 103.0 Appendix A A.4 Ergosterol, w /% ≤ 0.2 A.5 in Appendix A Specific rotation αm (20 ℃, D)/[(º) · dm2 · kg-1] 102.0 ~ 107.0 A.6 in Appendix A Mass absorption coefficient α (265nm)/(L/cm · g) 46 ~ 49 in Appendix A A.7 Reducing substance (tetrazolium color test), w /% ≤ 0.002 Appendix A A.8 Arsenic (As)/(mg/kg) ≤ 2 Appendix A A.9 Heavy metals (Pb)/(mg/kg) ≤ 20 Appendix A A.10

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, should be used with caution. If the Splashed on the skin should immediately wash with water, severe cases should be treated immediately. When using a volatile acid, to be carried out in a fume hood. A.2 General Provisions The reagents used in this standard, unless otherwise noted, only in the analysis confirmed analytically pure reagents and GB/T 6682-2008 in Regulation Given three water. Test methods used in the determination of impurities standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 602, GB/T 603 provisions of the preparation. A.3 Identification Test A.3.1 acetic anhydride concentrated sulfuric acid coloring test A.3.1.1 Reagents and materials A.3.1.1.1 chloroform. A.3.1.1.2 acetic anhydride. A.3.1.1.3 sulfuric acid. A.3.1.2 analysis step Laboratory samples taken from about 0.5 mg, after adding 5 mL chloroform dissolved, add 0.3 mL of acetic anhydride and 0.1 mL of sulfuric acid, shaking, previews yellow, Gradient red to purple immediately, and finally turns green. A.3.2 IR test Using potassium bromide tablet method according to GB/T 6040 test, IR spectra laboratory samples should be consistent (for the control of According to Atlas, see Appendix B). A.4 Determination of vitamin D2 A.4.1 Method summary By high performance liquid chromatography, under the selected operating conditions, the sample was separated by column chromatography with UV absorbance detector, With external standard method to calculate the content of the sample of vitamin D2. A.4.2 Reagents and materials A.4.2.1 pentanol. chromatography. A.4.2.2 hexane. chromatographically pure. A.4.2.3 isooctane. chromatography. A.4.2.4 vitamin D2 reference. A.4.2.5 vitamin D3 reference. A.4.3 Instruments and Equipment High performance liquid chromatography (HPLC). A.4.4 Chromatography conditions Recommended chromatographic columns and typical operating conditions are shown in Table A.1, vitamin D3 HPLC system suitability test diagram see Fig. C.1, the relative retention time of the components in Table C.1. Others can achieve the same degree of separation columns and chromatographic conditions can be used. Table A.1 column chromatography and typical operating conditions Column length 250mm, column diameter 4.6mm, silica gel column The mobile phase n-hexane - n-amyl alcohol (10 003) A flow rate of 2 mL/min Detector wavelength 254 nm A.4.5 Analysis step A.4.5.1 Preparation of vitamin D3 reference system suitability test stock solution Weigh about 25 mg of vitamin D3 reference, accurate to 0.000 1 g, brown set 100 mL volumetric flask, add 80 mL iso-octane, Sonication solubilization 1min, avoid heated to complete dissolution, coupled with iso-octane to the mark, shake nitrogen Mesa, dark, below 0 ℃ save. A.4.5.2 laboratory sample preparation solution It weighs about 25 mg laboratory samples, accurate to 0.000 1 g, brown set 100 mL volumetric flask, add 80 mL iso-octane, with Sonication solubilization 1min, avoid heated to complete dissolution, coupled with iso-octane to the mark. Measure 5 mL ± 0.05 mL above Solution, and placing 10 mL brown volumetric flask, add hexane to the mark. A.4.5.3 Preparation of standard solutions of Vitamin D2 Weigh about 25 mg of vitamin D2 reference, accurate to 0.000 1 g, brown set 100 mL volumetric flask, add 80 mL iso-octane, Sonication solubilization 1min, avoid heated to complete dissolution, coupled with iso-octane to the mark, amount of the above solution 5 mL ± 0.05 mL, Set 10 mL brown volumetric flask, add hexane to the mark. A.4.5.4 system suitability test Silica gel as a filler column, hexane - n-amyl alcohol (10 003) as the mobile phase, detection wavelength 254 nm, flow rate of about 2 mL/min. Amount of vitamin D3 reference substance stock solution 5 mL, set stoppered glass container, after nitrogen Mesa, set 90 ℃ water bath 1h, Remove rapid cooling, n-hexane 5 mL ± 0.05 mL, shake, set stoppered 1 cm quartz absorption cell in two main wavelengths of 254 nm And a 365 nm UV lamp, a quartz absorption cell diagonal 45 °, and from the tube 5 cm ~ 6 cm, irradiation 5min, the solution containing Provitamin D3, trans-vitamin D3, vitamin D3 and speed sterol D3. Of this solution into the liquid chromatograph to measure the peak of vitamin D3 Value, has injection five times the relative standard deviation should not exceed 2.0%, provitamin D3 (vitamin D3 than the retention time of 0.5) and Trans-vitamin D3 (vitamin D3 than the retention time of approximately 0.6) and vitamin D3 and D3-speed sterols (vitamin D3 retention ratio Time is about 1.1), a peak separation should be greater than 1.0. A.4.5.5 Determination Take 20μL laboratory sample solution into the liquid chromatograph, record the chromatograms, the other to take vitamin D2 reference solution, the same method. By external standard method to calculate the peak area of the test content of vitamin D2. A.4.6 Calculation Results Vitamin D2 calculated in accordance with the chromatogram mass fraction w1, expressed in%, according to formula (A.1) Calculation 100% m Aw A m × = ×× (A.1) Where. 1m - injection volume values of the reference solution of vitamin D2, in micrograms (μg); 2A - Numerical laboratory sample solution of vitamin D2 peak area; 1A - vitamin D2 Numerical control solution peak area; 2m - laboratory sample solution injection amount of vitamin D2 values, in micrograms (μg). Take two parallel determination results of the arithmetic average of the measurement results, the two parallel determination allows absolute difference is not more than 1.5%. A.5 Determination of ergosterol A.5.1 Method summary Vitamin D2 solution was spotted on a TLC plate, if commenced, after the color, the chromatogram obtained with reference solution obtained by the same method Chromatograms for comparison, vitamin D2 impurity inspection. A.5.2 Reagents and materials A.5.2.1 squalane chloroform solution. 10 g/L. A.5.2.2 developing solvent. cyclohexane - ether (11). A.5.2.3 vitamin D2 reference. A.5.2.4 ergosterol reference. A.5.3 Analysis step A.5.3.1 preparation of the reference solution Weigh about 50 mg of vitamin D2 reference, accurate to 0.000 2 g, with 1 mL of squalane was dissolved in chloroform solution, was the reference solution liquid. A.5.3.2 laboratory sample preparation solution Weigh about 50 mg of vitamin D2 laboratory samples, accurate to 0.000 2 g, with 1 mL of squalane was dissolved in chloroform to give the laboratory sample Solution. A.5.3.3 ergosterol control solution preparation Weigh about 5 mg ergosterol reference to the nearest 0.1 mg, placed in 50 mL volumetric flask, add squalane chloroform solution 40 mL solution Solution and diluted to the mark. A.5.3.4 was formulated toner Take 1.0 g antimony trichloride, add 20 mL of acetyl chloride dissolved. A.5.3.5 Determination Were taken 10 μL standard solutions, laboratory sample solution and control solution ergosterol, respectively, point to sodium carboxymethyl cellulose Adhesive silica gel G plate, with the developing solvent in the dark started to dry, color chromogenic agent. Laboratory sample solution and reference solution Liquid main spot Rf value and the color should be consistent, impurity spots laboratory sample solution can not be deeper than the control solution ergosterol appropriate spots. A.6 Determination of specific rotation A.6.1 Reagents and materials Ethanol. A.6.2 Instruments and Equipment Polarimeter. A.6.3 Analysis step Take the right amount of laboratory samples, accurate to 0.000 2 g, add ethanol made from 1 mL containing about 40 mg of the solution, the other in GB/T 613-2007 method prescribed conduct. (Note. Determination within 30min after the solution preparation). A.6.4 Calculation Results Specific rotation аm (20 ℃, D) according to the formula (A.2) Calculated. () 20, m CD l αα ρ∂ ° = × (A.2) Where. α - measured angle of rotation, in degrees (°); l - the length of the optical tube unit decimeter (dm); αρ - mass concentration in the solution effective component in grams per milliliter (g/mL). Determination A.7 mass absorption coefficient A.7.1 Reagents and materials Ethanol. A.7.2 Instruments and Equipment UV spectrophotometer. A.7.3 Analysis step Weigh the right amount of laboratory samples, accurate to 0.000 2 g, add ethanol produced per 1 mL containing about 10 μg of the sample solution, according to GB/T 9721 at a wavelength of 265 nm ± 1 nm measured absorbance A, seeking the mass absorption coefficient. A.7.4 Calculation Results The absorption coefficient α calculated based on the absorbance A mass of vitamin D2, numerical order (º) · dm2 · kg-1 according to formula (A.3) Calculated. b α α ρ = × (A.3) Where. A-- absorbance value of the sample solution; b - the optical path length (i.e. the thickness of the absorption cell) values in centimeters (cm & lt); αρ - laboratory sample solution concentration values in grams per liter (g/L). A.8 Determination of reducing substances A.8.1 principle of the method Reducing substances can in strong alkaline solution tetrazolium reduction colored formazan (formazan), and toluene ethanol also diphenols Standard color of the solution of the original substance is relatively limited examination do. A.8.2 Reagents and materials A.8.2.1 ethanol. A.8.2.2 methanol. A.8.2.3 glacial acetic acid. A.8.2.4 tetrazolium methanol solution. 50 mg/mL. A.8.2.5 tetramethylammonium hydroxide solution. an aqueous solution of tetramethylammonium hydroxide (100 g/L) - ethanol (19). A.8.2.6 A diphenol of absolute ethanol. 0.2 μg/mL. A.8.3 Analysis step A.8.3.1 laboratory sample preparation solution Weigh about 0.1 g laboratory samples, accurate to 0.001 g, was dissolved in absolute ethanol, diluted to 10 mL, 0.5 mL of blue tetrazolium Methanol solution and 0.5 mL of tetramethylammonium hydroxide solution, standing 5min, added 1.0 mL of glacial acetic acid, shake. A.8.3.2 control solution preparation Measure 10 mL ± 0.05 mL 0.2 μg/mL of methyl diphenol absolute ethanol was added 0.5 mL of methanol four tetrazolium solution and 0.5 mL hydroxyl Tetramethylammonium solution was allowed to stand 5min, added 1.0 mL of glacial acetic acid, shake. A.8.3.3 Preparation of blank solution Take 10 mL of absolute ethanol was added 0.5 mL of methanol solution of tetrazolium and 0.5 mL tetramethylammonium hydroxide solution, standing 5min, added 1.0 mL glacial acetic acid, shake. A.8.3.4 Determination At 525 nm wavelength, with zero blank solution, were measured absorbance of the sample solution and control solution laboratory, laboratory sample The absorbance of the solution should not be greater than the control solution. A.9 Determination of Arsenic Take 5 g ± 0.01 g laboratory samples, dry ashing process samples. Take the same amount of magnesium oxide, magnesium nitrate and sample the same treatment, Reagent blank test. Measure 10 mL ± 0.05 mL of arsenic standard solution (arsenic 2.0μg), with treatment, the preparation of arsenic limits. press The provisions of GB/T 5009.76-2003 Gutzeit method performed. A.10 Determination of Heavy Metals A.10.1 reagents and materials A.10.1.1 nitrate. A.10.1.2 sulfuric acid. A.10.1.3 hydrochloric acid. A.10.1.4 glycerol. A.10.1.5 ammonium acetate. A.10.1.6 lead nitrate. A.10.1.7 thioacetamide. A.10.1.8 ammonia solution. 400 → 1000. A.10.1.9 sodium hydroxide solution. c (NaOH) = 1 mol/L. A.10.1.10 hydrochloric acid solution. c (HCl) = 2 mol/L. A.10.1.11 hydrochloric acid solution. c (HCl) = 7 mol/L. A.10.1.12 ammonia solution. c (NH3 · H2O) = 5 mol/L. A.10.1.13 phenolphthalein indicator solution. 10g/L ethanol solution. A.10.1.14 acetate buffer (pH3.5). Take 25 g of ammonium acetate, 25 mL water was added after dissolved, and 7 mol L hydrochloric acid/38 mL, PH was adjusted to accurately 3.5 of 5 (pH meter) with 2 mol/L aqueous ammonia solution or hydrochloric acid solution, dilute with water to 100 mL. A.10.1.15 thioacetamide test solution. Take 4 g thioacetamide, to the nearest 0.01 g, add water to dissolve into a 100 mL, set the refrigerator Mediator Deposit. Immediately prior to taking 5.0 mL mixture (by a 1 mol/L 15 mL of sodium hydroxide solution, 5.0 mL of water and 20 mL glycerol), plus the above 1.0 mL of thioacetamide solution was heated on a water bath 20s, cooling, use immediately. A.10.1.16 lead standard solution. Weigh 0.160 g of lead nitrate, accurate to 0.000 2g, placed in 1000 mL volumetric flask, add 5 mL of nitric acid After dissolution with 50 mL of water, dilute to the mark, shake, as the stock solution. Before use, Pipette (10 ± 0.02) mL stock solution, Placed 100 mL volumetric flask, diluted with water to the mark, shake, that was (per 1mL equivalent to 10 μg of Pb). And storage configuration used Glassware shall lead. A.10.2 Analysis steps Press the "People's Republic of China Pharmacopoeia" 2005 edition Appendix Ⅷ H Method II test for heavy metals, as follows. Take 1 g ± 0.01 g laboratory samples, slowly burn to completely carbonized, let cool, add 0.5 mL ~ 1.0 mL of sulfuric acid, so just moist, Divisible by low-temperature heating sulfuric acid, add 0.5 mL of nitric acid, evaporated to oxide vapor divisible after allowing to cool, 500 ℃ ± 50 ℃ in Chi Burn to completely gray, let cool, add 2 mL of hydrochloric acid, add 15 mL water was evaporated on a water bath set, dropping ammonia solution to phenolphthalein instructions VIS Neutral, plus 2 mL acetate buffer (pH3.5), after heat gently to dissolve, displacing Nessler colorimetric tube A tube, diluted with water to 25 mL; Another laboratory sample preparation reagent solution, evaporated to dryness rear porcelain dish, add 2 mL acetate buffer (pH 3.5) and 15 mL of water, After heat gently to dissolve, displacing Nessler colorimetric tube acetate tube, add 2 mL ± 0.02 mL lead standard solution, and then diluted with water to 25 mL; then in the armor B two respectively, plus 2 mL thioacetamide test solution, shake 2min, on the same set of paper, from the top down perspective, A tube was B color tube shown in comparison with, not deeper.

Appendix B

(Normative) IR spectra Vitamin D2 Note. Quoted from "Drug IR set," Volume I (1995) Figure B.1 IR spectra of vitamin D2

Appendix C

(Informative) System suitability test performance liquid chromatogram and relative retention times Figure C.1 Figure HPLC system suitability test Table C.1 each peak retention time and relative retention times Ingredient name order peak relative retention time 1 solvent peak - 2,3 unknown peaks - 4 provitamin D3 0.54 5-trans vitamin D3 0.60 6 Vitamin D3 1.00 7-speed sterol D3 1.11 ......

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