GB 29942-2013Food additive -- Vitamin E (dl-tocopherol) (English PDF)

2.1 Chemical Name

dl-2,5,7,8- tetramethyl-2- (4,8,12-trimethyl - tridecyl) -6-chromanol ol Formula 2.2 C29H50O2

2.3 Formula

OCH3

CH3

CH3 CH3 H HCH3 CH3 CH3 CH3

2.4 Relative molecular mass

430.71 (according to 2007 international relative atomic mass)

3.1 Sensory requirements

Sensory requirements shall comply with the requirements of Table 1.

Table 1 Sensory requirements

Project requires test methods Pale yellow to amber color, exposure to air or light color becomes deep porcelain drip proper amount of sample was placed on the board, in natural light the line, observe its color and clear viscous liquid state status

3.2 Physical and Chemical Indicators

Physical and chemical indicators should be consistent with the provisions of Table 2.

Table 2. Physical and chemical indicators

Item Index Test Method Vitamin E (dl-alpha- tocopherol) content, w /% 96.0 ~ 102.0 Appendix A A.3 Refractive index 20Dn 1.503 ~ 1.507 GB/T 614 Absorbance) (nm292 m1E 71 ~ 76 in Appendix A A.4 Residue on ignition, w /% <= 0.1 GB/T 9741 by acidity test A.5 in Appendix A Lead (Pb)/(mg/kg) <= 2 GB 5009.12 Appendix A Testing method A.1 General Provisions Unless otherwise specified in this standard, the use of analytical reagent purity should be more than the standard titration solution, standard solution for measuring impurities, Preparations and products, should be GB/T 601, GB/T 602, GB/T 603 requirements preparation, test water should be consistent with GB/T 6682-2008 in three Water provisions. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution.

A.2 Identification Test A.2.1 solubility Insoluble in water, soluble in ethanol, miscible in ether.

A.2.2 Specific rotation test A.2.2.1 Reagents and materials Chloroform. chromatography.

A.2.2.2 instruments and equipment Polarimeter.

A.2.2.3 analysis step Weigh the sample 5.0 g, add chloroform to dissolve and dilute to 50 mL, the sample solution is placed in this polarimeter in determination, specific analysis step Step according to the provisions GB/T 613 will be. The measured specific rotation alpham (20 °C, D) should be 0 (°) · dm2 · kg-1 ± 0.05 (°) · dm2 · kg-1.

A.2.3 nitric acid coloring test A.2.3.1 Reagents and materials A.2.3.1.1 ethanol.

A.2.3.1.2 nitrate.

A.2.3.2 analysis step Weigh a sample of about 10 mg, dissolved add 10 mL of anhydrous ethanol, add 2 mL of nitric acid, shaken, and heated at 75 °C water bath for 15 min, the solution it should exhibit bright red to orange.

The maximum absorption wavelength A.2.4 Test A.2.4.1 instruments and equipment UV spectrophotometer.

A.2.4.2 analysis step Weigh the sample 0.01 g, add ethanol dissolved and diluted to 200 mL, shake, placed in the scanning UV spectrophotometer at 292 nm ± 2 nm at the maximum absorption peak due.

A.3 Determination of Vitamin E (dl-alpha- tocopherol) Content A.3.1 Method summary by gas chromatography, under the selected operating conditions, the non-polar silica capillary columns by the sample and separation of impurities with hydrogen flame Ionization detector and quantified using internal standard, the sample is calculated vitamin E (dl-alpha- tocopherol) content.

A.3.2 Reagents and materials A.3.2.1 hexane. chromatographically pure.

A.3.2.2 palmitic acid cetyl alcohol esters.

A.3.2.3 Vitamin E (dl-alpha- tocopherol) standard.

A.3.2.4 Vitamin E (dl- alpha- tocopheryl acetate) standard.

A.3.3 Instruments and Equipment Gas chromatograph with flame ionization detector.

A.3.4 reference chromatographic conditions A.3.4.1 Column. length 30 m, column diameter 0.25 mm, stationary phase polydimethylsiloxane, a thickness of 0.25 µm.

A.3.4.2 Column temperature. 280 °C.

A.3.4.3 Detector. flame ionization detector, temperature 290 °C.

A.3.4.4 Inlet. temperature 290 °C; split injection, split ratio 1.30; injection volume was 1 µL.

A.3.4.5 carrier gas. nitrogen, flow rate of 1 mL/min.

A.3.4.6 A.3.4.1 ~ A.3.4.5 recommended chromatographic column and typical operating conditions, dl-alpha- tocopherol determination typical GC

Figure in Appendix B. Other to achieve equivalent separation columns and chromatographic conditions can be used.

A.3.5 Analysis step

A.3.5.1 Preparation of internal standard solution Weighed amount of palmitic acid ester of cetyl alcohol (internal standard), adding hexane to dissolve, dilute, shake, as the internal standard solution. This internal standard solution per ml L containing 3 mg palmitic acid cetyl alcohol esters.

A.3.5.2 Preparation of standard solutions it weighs about 30 mg of vitamin E (dl-alpha- tocopherol) standard, accurate to 0.000 1 g, placed in 10 mL brown volumetric flask, add internal standard solution Was dissolved and diluted to the mark, shake, as the standard solution.

A.3.5.3 Preparation of sample solution Weigh about 30 mg samples, accurate to 0.000 1 g, placed in 10 mL brown volumetric flask, add internal standard solution to dissolve and dilute to volume, shake Even as the sample solution.

A.3.5.4 system suitability test Weigh the same amount of vitamin E (dl-alpha- tocopherol) standard and vitamin E (dl-alpha- tocopheryl acetate) standard, add n-hexane solution Solution, formulated as per milliliter of n-hexane containing respectively 1 mg of vitamin E (dl-alpha- tocopherol) standard and 1 mg of vitamin E (dl-alpha- tocopherol acetate) A mixed solution standard. In A.3.4 reference chromatographic conditions, multiple injections, the mixed solution was subjected to chromatographic analysis, measurement resolution R, R should not less than 3.

A.3.5.5 Instrument calibration in A.3.4 reference chromatographic conditions, take A.3.5.2 standard solution consecutive injections until three consecutive needle relative response factor f is a constant (relative Deviation within 2%). According to the standard retention time qualitative measurement of vitamin E (dl-alpha- tocopherol) and the internal standard peak area, the phase the corresponding values were recorded as AS and AP. According to formula (A.1) to calculate the relative response factor f.

A.3.5.6 Determination of content Amount of 1.0 µL sample solution is injected into the gas chromatograph, record the chromatograms, and measure the vitamin E (dl-alpha- tocopherol) and the peak area of internal standard, the corresponding values recorded as A2 and A1. According to formula (A.2) calculates the sample of vitamin E (dl-alpha-- tocopherol) content.

A.3.5.7 Calculation Results A.3.5.7.1 relative response factor Relative response factor f according to formula (A.1) Calculated.

Af x= (A.1)

Where.

AS-- standard solution chromatogram of vitamin E (dl-alpha- tocopherol), a peak area value;

Peak area in the chromatogram of the standard solution AP-- standard material;

MP-- quality standards within the standard material solution, in milligrams (mg);

Quality mS-- standard solution of vitamin E (dl-alpha- tocopherol), in units of milligrams (mg).

A.3.5.7.2 content

Vitamin E (dl-alpha- tocopherol) content of the mass fraction w1 according to formula (A.2) Calculated.

twenty one

1 xxx= mA

mw (A.2)

Where.

Quality in the specimen solution m1-- standard material, in milligrams (mg);

f-- relative response factor;

A2-- chromatogram of the sample solution of vitamin E (dl-alpha- tocopherol), a peak area value;

Peak area in the chromatogram of the sample solution A1-- standard material;

Quality m0-- sample, in milligrams (mg).

The results parallel arithmetic mean of the measurement results shall prevail. Two independent determination results obtained under the repeatability condition of absolute difference not more than 2% of the arithmetic mean.

A.4 Determination of absorbance A.4.1 Reagents and materials Ethanol.

A.4.2 Instruments and Equipment Spectrophotometer.

A.4.3 Analysis step

Weigh about 0.01 g samples, accurate to 0.002 g, add ethanol dissolved and diluted to 200 mL, shake to obtain a sample solution. Take this sample Was placed in a 1 cm cuvette, anhydrous ethanol as blank, absorbance was measured at 292 nm with a spectrophotometer at (absorbance should be controlled Between 0.2 and 0.8, or the concentration of the sample should be adjusted, and re-measured absorbance).

A.4.4 Calculation Results Absorbance) (nmE cm 292 according to formula (A.3) Calculated.

1) 292 (m1 x= c

AnmE (A.3)

Where.

A-- absorbance of the sample solution to be tested;

c-- concentration of the sample solution to be tested, in grams per milliliter (g/mL);

100-- concentration conversion factor.

The results parallel arithmetic mean of the measurement results shall prevail. Two independent determination results obtained under the repeatability condition of absolute difference the ratio of the arithmetic mean of less than 2%.

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 phenolphthalein indicator solution. 10 g/L.

A.5.1.4 sodium hydroxide standard titration solution. c (NaOH) = 0.1 mol/L.

A.5.2 Analysis step

Amount of ethanol and ether each 12.5 mL, placed in a conical flask, dubbed a mixed solution of sodium hydroxide standard titration solution, titration to phenol Phthalate indicator solution indicates the solution is neutral. Weigh 1.0 g sample was added Erlenmeyer flask, and dissolved, together with 0.5 mL of phenolphthalein indicator solution, and then Sodium hydroxide standard titration solution, titration, until the solution was pale pink, do not fade within 30 s, is the titration end point. After recording plus sample consumption the volume of sodium hydroxide standard titration solution. The required volume of sodium hydroxide standard titration solution is not more than 1.0 mL sample through the test.

Appendix B

Determination of vitamin E (dl-alpha- tocopherol) content of a typical gas chromatogram Determination of vitamin E (dl-alpha- tocopherol) content of a typical gas chromatography is shown in Figure B.1.

1-- solvent (n-hexane);

2-- Vitamin E (dl-alpha- tocopherol);

3-- internal standard (palmitic acid cetyl alcohol esters).

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