GB 14756-2010National food safety standards -- Food additives -- Vitamin E (dl-alpha-acetate tocopherol) (English PDF)

Foreword

This standard replaces GB 14756-1993 "Food additive vitamin E (dl-alpha- tocopheryl acetate)." this standard compared with GB 14756-1993, the main changes are as follows.

- Cancel the ferric chloride color reaction bipyridine project identification and the corresponding test methods;

- An increase of infrared absorption spectroscopy to identify the project and the corresponding test methods;

- Modify the determination of vitamin E;

- Modify the determination of heavy metals.

Appendix A of this standard is a normative appendix, Appendix B is an informative annex.

This standard replaces the standards previously issued as follows.

--GB 14756-1993.

National Food Safety Standard Food additives Vitamin E (dl-alpha- tocopherol acetate)

1 Scope

This standard is suitable for use by the trimethylhydroquinone and isophytol as raw material by chemical synthesis of food additives vitamin E (Dl-alpha- tocopheryl acetate).

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, only the date of the note Stage version applies to this standard. For undated references, the latest edition (including any amendments) are applicable to this standard quasi.

3 Chemical name, molecular formula, molecular mass and structural formula

4 Technical Requirements

4.1 Sensory requirements. comply with Table 1.

Table 1 Sensory requirements

Project requires test methods Color yellow to yellow or yellow-green, the case of light color gradient depth 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 almost odorless Clear viscous liquid state organization

4.2 Physical indicators. to comply with Table 2.

Table 2. Physical and chemical indicators

Item Index Test Method Vitamin E (C31H52O3), w /% 96.0 ~ 102.0 Appendix A A.4 <= acidity test by test A.5 in Appendix A Heavy metals (Pb)/(mg/kg) <= 10 Appendix A A.6 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 splashed on the skin should immediately wash with water, severe cases should be treated immediately. When using a volatile acid, to be in the hood.

A.2 General Provisions Unless otherwise indicated in the analysis using only confirm three analytical grade reagents and water GB/T 6682-2008 stipulated.

The test method used in the standard titration solution, impurity measurement standard solution, preparations and products, not specified in other requirements, are According to GB/T 601, GB/T 602, GB/T 603 provisions of the preparation.

A.3 Identification Test A.3.1 nitric acid coloring test A.3.1.1 Reagents and materials A.3.1.1.1 ethanol.

A.3.1.1.2 nitrate.

A.3.1.1.3 vitamin E reference.

A.3.1.2 analysis step Weigh about 30 mg laboratory samples, after adding 10 mL of anhydrous ethanol dissolved, add 2 mL of nitric acid, shaken, and heated at 75 °C 15 min, Orange-red solution should be obvious.

A.3.2 infrared absorption spectrum test Using potassium bromide smear, according to GB/T 6040 infrared absorption spectrum, infrared spectrum should be measured with reference vitamin E the spectrum.

A.4 Determination of vitamin E A.4.1 Method summary by gas chromatography, under the selected operating conditions, the non-polar silica capillary columns by contacting the sample with separation of impurities with hydrogen Flame ionization detector, with the internal standard method to calculate the vitamin E content in the sample.

A.4.2 Reagents and materials A.4.2.1 hexane. chromatographically pure.

A.4.2.2 palmitic acid cetyl alcohol esters.

A.4.2.3 vitamin E reference.

A.4.3 Instruments and Equipment Gas Chromatograph.

A.4.4 Chromatography conditions Recommended chromatographic columns and typical operating conditions are shown in Table A.1, vitamin E (dl-alpha- tocopheryl acetate) Determination Typical Gas See Appendix B in the chromatogram Figure B.1, relative retention time of the components in Appendix B, Table B.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 30 m, column diameter 0.53 mm or 0.32 mm, fixative is 100% methyl polysiloxane Column temperature 280 °C Detector flame ionization detector, a temperature of 300 °C Inlet temperature of 290 °C; split injection, split ratio of 1.20; 1 µL injection volume Nitrogen carrier gas flow rate of 5 mL/min A.4.5 Analysis step A.4.5.1 Preparation of internal standard solution Weigh palmitic acid ester of cetyl alcohol amount, add n-hexane was dissolved, diluted per 1 mL solution containing 3 mg cetyl alcohol, palmitic acid esters, shake Even as the internal standard solution.

A.4.5.2 Preparation of the reference solution Weigh about 30 mg of vitamin E reference, accurate to 0.000 1 g, set 10 mL brown volumetric flask, add internal standard solution to dissolve and Diluted to the mark, shake, as the reference solution.

A.4.5.3 Preparation of sample solution Weigh about 30 mg laboratory samples, accurate to 0.000 1 g, set 10 mL brown volumetric flask, add internal standard solution and diluted to the mark, shake, as a sample solution.

A.4.5.4 system suitability test with methyl silicone as the stationary phase of silica capillary column (30 m × 0.53 mm), column temperature of 280 °C, number of theoretical plates for a living Vitamin E shall be not less than 3000, and the separation of vitamin E and the internal standard peak should be greater than 3.

Determination A.4.5.5 Content 1.0µL weighed sample solution into the gas chromatograph, record the chromatograms, another reference solution, the same method. According to the internal standard peak Calculate the area of content in the sample C31H52O3.

A.4.6 Calculation Results Vitamin E (C31H52O3) content mass fraction w1, expressed in%, according to the formula (A.1), (A.2) Calculated.

mAfw% (A.1)

twenty one

mAf ×

Where.

f - relative correction factor of vitamin E;

A1 - Numerical control solution of the standard substance peak area;

A2 - the value of vitamin E in the reference solution peak area;

A3 - the value of vitamin E in the sample solution peak area;

A4 - Numerical solution of the sample peak area of the standard;

m1 - the quality of internal control solution in standard material values, in milligrams (mg);

m2 - mass value of vitamin E in the reference solution, in milligrams (mg);

m3 - mass of the sample solution in the sample values in milligrams (mg);

m4 - numerical solution of the internal standard sample mass, in milligrams (mg).

Take two parallel determination results of the arithmetic average of the measurement results, the results of two parallel determination of the absolute difference is not more than 1.5%.

A.5 Determination of acidity 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) = 0.1 mol/L.

A.5.1.4 phenolphthalein indicator solution. 10 g/L ethanol solution.

A.5.2 Analysis step

Amount of ethanol and 15 mL, respectively, ether, set conical flask, add 0.5 mL of phenolphthalein indicator solution, a solution of sodium hydroxide standard titration Solution to pale pink color, after adding 1.0 g laboratory sample is dissolved, titrated with sodium hydroxide standard titration solution, sodium hydroxide consumed drop Given solution is not more than 0.5 mL by experiment.

A.6 Determination of Heavy Metals A.6.1 Reagents and materials A.6.1.1 nitrate.

A.6.1.2 sulfuric acid.

A.6.1.3 hydrochloric acid.

A.6.1.4 glycerol.

A.6.1.5 ammonium acetate.

A.6.1.6 lead nitrate.

A.6.1.7 thioacetamide.

A.6.1.8 ammonia solution. 400 -> 1000.

A.6.1.9 sodium hydroxide solution. c (NaOH) = 1 mol/L.

A.6.1.10 hydrochloric acid solution. c (HCl) = 2 mol/L.

A.6.1.11 hydrochloric acid solution. c (HCl) = 7 mol/L.

A.6.1.12 ammonia solution. c (NH3 · H2O) = 5 mol/L.

A.6.1.13 phenolphthalein indicator solution. 10g/L ethanol solution.

A.6.1.14 acetate buffer (pH3.5).

Take 25 g of ammonium acetate, add 25 mL of water to dissolve, plus 7 mol L hydrochloric acid/38 mL, with 2 mol/L hydrochloric acid solution or aqueous ammonia solution Accurate pH was adjusted to 3.5 (pH meter), diluted to 100 mL.

A.6.1.15 thioacetamide test solution.

Take 4 g thioacetamide, to the nearest 0.01 g, add water to dissolve into a 100 mL, home refrigerator. Immediately prior to taking 5.0 mL mixed A mixed solution [15 mL from the sodium hydroxide solution, 5.0 mL of water and 20 mL glycerol], plus the aforementioned 1.0 mL of thioacetamide solution, a water bath on heating 20s, cooling, use immediately.

A.6.1.16 lead standard solution.

Weigh 0.160 g of lead nitrate, accurate to 0.000 2 g, placed in 1000 mL volumetric flask, add 5 mL and 50 mL of nitric acid dissolved in water, Diluted with water to the mark, shake, as the stock solution. Before use, pipette 10 mL ± 0.02 mL stock solution into 100 mL volumetric flask, Diluted with water to the mark, shake, that was (per 1mL equivalent to 10 µg of Pb). Configuration and glassware used for storage shall lead.

A.6.2 Analysis step

Press the "People's Republic of China Pharmacopoeia" 2005 edition Appendix VIII H second method for the determination of heavy metals Inspection Act, as follows.

Weigh 1.0 g ± 0.01 g laboratory samples, set in the crucible slowly burn to completely carbonized, let cool; add 0.5 mL sulfuric acid so moist, low Heated to a temperature of sulfuric acid vapor divisible after, at 500 °C ~ 600 °C ignition completely gray, displaced within the dryer, let cool, take the residue left over, Nitrate plus 0.5 mL, evaporated to oxide vapor divisible After cooling, hydrochloric acid 2 mL, add water evaporated on a water bath 15 mL, dropping Ammonia solution to phenolphthalein instructions VIS neutral, together with acetate buffer (pH3.5) 2 mL, after heat gently to dissolve, displacing Nessler colorimetric tube A Tube, diluted with water to 25 mL; Another solution prepared for the test reagents, then to porcelain dish evaporated, add acetate buffer (pH3.5) 2 mL and water 15 mL, after heat gently to dissolve, displacing Nessler colorimetric tube acetate tube, add lead standard solution 1.0 mL, and then diluted with water to 25 mL;

And then were added to the two B thioacetamide test solution in each of 2 mL, shake, place 2 min, on the same set of paper, from the top down perspective, armor B color comparison tube tube display and no deeper.

Appendix B

(Informative)

Vitamin E (dl-alpha- tocopheryl acetate) Determination of a typical gas chromatogram of each component and the relative retention time 1-- solvent (n-hexane) 2 - Vitamin E (dl-alpha- tocopherol acetate) 3 - internal standard (cetyl alcohol, palmitic acid ester)

Figure B.1 Determination of Vitamin E (dl-alpha- tocopheryl acetate) content of a typical gas chromatogram

Table B.1 Determination of Vitamin E (dl-alpha- tocopheryl acetate) content of each component relative retention time

Ingredient name order peak relative retention time (min) 1 hexane 0.03 2 vitamin E 1.00 3 internal standard (cetyl alcohol, palmitic acid ester) 1.49 Peak area