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GB 29942-2013: Food additive -- Vitamin E (dl-tocopherol)
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Food additive -- Vitamin E (dl-tocopherol)
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GB 29942-2013
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Basic data
| Standard ID | GB 29942-2013 (GB29942-2013) |
| Description (Translated English) | Food additive -- Vitamin E (dl-tocopherol) |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C54 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 11,122 |
| Regulation (derived from) | China Food & Drug Administration [2013] No. 234, November, 1, 2013 |
| Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China |
| Summary | This standard applies to food additives: vitamin E (dl tocopherol). |
GB 29942-2013: Food additive -- Vitamin E (dl-tocopherol)
---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.
Food additive-Vitamin E (dl-tocopherol)
National Standards of People's Republic of China
Issued on. 2013-11-29
2014-06-01 implementation
National Food Safety Standard
Food additives Vitamin E (dl-α- tocopherol)
National Food Safety Standard
Food additives Vitamin E (dl-α- tocopherol)
1 Scope
This standard applies to different plant alcohol trimethyl hydroquinone as the main raw material, chemical synthesis of food additives, vitamin E (dl-α-
Tocopherol).
2 chemical name, molecular formula, molecular mass and structural formula
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
OH
CH3
CH3 CH3 H HCH3 CH3 CH3
CH3
2.4 relative molecular mass
430.71 (according to 2007 international relative atomic mass)
3 Technical requirements
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-α- 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 αm (20 ℃, D) should be 0 (º) · dm2 · kg-1 ± 0.05 (º) · 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 ℃ 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-α- 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-α- 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-α- tocopherol) standard.
A.3.2.4 Vitamin E (dl- α- 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. 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 ℃.
A.3.4.3 Detector. flame ionization detector, temperature 290 ℃.
A.3.4.4 Inlet. temperature 290 ℃; 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-α- 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-α- 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-α- tocopherol) standard and vitamin E (dl-α- tocopheryl acetate) standard, add n-hexane solution
Solution, formulated as per milliliter of n-hexane containing respectively 1 mg of vitamin E (dl-α- tocopherol) standard and 1 mg of vitamin E (dl-α- 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-α- 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-α- 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-α-- 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 (A.1)
Where.
AS-- standard solution chromatogram of vitamin E (dl-α- 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-α- tocopherol), in units of milligrams (mg).
A.3.5.7.2 content
Vitamin E (dl-α- tocopherol) content of the mass fraction w1 according to formula (A.2) Calculated.
twenty one
1 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-α- 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 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, 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-α- tocopherol) content of a typical gas chromatogram
Determination of vitamin E (dl-α- tocopherol) content of a typical gas chromatography is shown in Figure B.1.
1-- solvent (n-hexane);
2-- Vitamin E (dl-α- tocopherol);
3-- internal standard (palmitic acid cetyl alcohol esters).
Figure B.1 Determination of Vitamin E (dl-α- tocopherol) content of a typical gas chromatogram
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