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GB 1886.233-2016: Food additive -- Natural vitamin E
GB 1886.233-2016
NATIONAL STANDARD OF THE
PEOPLE?€?S REPUBLIC OF CHINA
National Food Safety Standard -
Food Additive - Vitamin E
ISSUED ON: AUGUST 31, 2016
IMPLEMENTED ON: JANUARY 1, 2017
Issued by: National Health and Family Planning Commission of the PRC
Table of Contents
Foreword ... 3
1 Application Scope ... 4
2 Chemical Name, Molecular Formula, Structural Formula and Relative Molecular
Mass ... 4
3 Technical Requirements ... 6
Appendix A Test Method ... 8
National Food Safety Standard -
Food Additive - Vitamin E
1 Application Scope
This standard applies to natural vitamin E extracted from by-products of natural edible
vegetable oil or synthetic vitamin E, and products prepared from edible vegetable oil.
Vitamin E applicable to this standard includes the following tocopherol types: d-??-
tocopherol, dl-??-tocopherol, d-??-tocopheryl acetate, dl-??-tocopheryl acetate, d-??-
tocopheryl acid succinate, dl-??-tocopheryl acid succinate, d-??-tocopheryl acetate
concentrate and mixed tocopherols concentrate.
2 Chemical Name, Molecular Formula, Structural Formula
and Relative Molecular Mass
2.1 Chemical name
d-??-tocopherol: (+) 2,5,7,8-tetramethyl 2-(4,8,12-trimethyltridecyl) 6-chromanone;
dl-??-tocopherol: (??) 2,5,7,8-tetramethyl 2-(4,8,12-trimethyltridecyl) 6-chromanol;
d-??-tocopheryl acetate: (+) 2,5,7,8-tetramethyl 2-(4,8,12-trimethyltridecyl)
benzopyran-6-acetate;
dl-??-tocopheryl acetate: (??) 2,5,7,8-tetramethyl 2-(4,8,12-trimethyltridecyl) 6-
benzohydropyranol acetate;
d-??-tocopheryl acid succinate: (+) 2,5,7,8-tetramethyl 2-(4,8,12-trimethyltridecyl)
chromool 6-succinate;
dl-??-tocopheryl acid succinate: (??) 2,5,7,8-tetramethyl 2-(4,8,12-trimethyltridecyl)
chromanol 6-succinate.
2.2 Molecular formula
d-??-tocopherol: C29H50O2
dl-??-tocopherol: C29H50O2
d-??-tocopheryl acetate: C31H52O3
Appendix A
Test Method
A.1 General provisions
Unless otherwise specified in this standard, the purity of reagents used shall be above
the grade of analytical reagent; the used standard titration solutions, the standard
solutions for the determination of impurities, the preparations and products shall be
prepared in accordance with the provisions of GB/T 601, GB/T 602 and GB/T 603; the
test water should meet the requirements of grade-3 water specified by GB/T 6682.
The solution used in the test, if not indicated which solvent is used, refers to aqueous
solution.
A.2 Identification test
A.2.1 Reagents and materials
A.2.1.1 Absolute ethanol.
A.2.1.2 Nitric acid.
A.2.2 Identification method
A.2.2.1 Take about 50 mg of sample; add 10 mL of absolute ethanol to dissolve; shake;
add 2 mL of nitric acid; heat at 75??C for 15 min; then the color is shown light red to
orange.
A.2.2.2 On the gas chromatogram of content determination, the main peak of the
sample solution (mixed tocopherol should be the third main peak) should be consistent
with the retention time of the main peak of the reference solution (except solvent peak
and internal standard peak).
A.3 Content determination
A.3.1 Reagents and materials
A.3.1.1 Cetyl palmitate.
A.3.1.2 ??-tocopherol reference substance.
A.3.1.3 ??-tocopheryl acetate reference substance.
A.3.1.4 ??-tocopheryl acid succinate reference substance.
A.3.1.5 n-hexane.
Where:
Aint1 -- internal standard peak area;
????????? ??? -- the concentration of ??-tocopherol reference substance, in milligrams per
milliliter (mg/mL);
Aref1 -- ??-tocopherol peak area;
??int1 -- internal standard concentration of the internal standard solution, in milligrams
per milliliter (mg/mL).
A.3.3.1.4 Determination
Inject 1 ??L of the sample solution into the gas chromatograph; record the
chromatogram; calculate the peak area of ??-tocopherol, ??- and ??-tocopherol, and ??-
tocopherol (A??2, A??,??2, A??2); calculate the sum of the first three items (At2) and the
internal standard peak area Aint2; calculate the content according to Formula (A.2) and
Formula (A.3):
Where:
f1 -- correction factor;
At2 -- total peak area of tocopherol peak;
??int1 -- internal standard solution concentration, in milligrams per milliliter (mg/mL);
Aint2 -- internal standard peak area;
????????????????????? -- concentration of the sample solution, in milligrams per milliliter (mg/mL);
wref - content of ??-tocopherol reference substance, %.
Aa2 -- ??-tocopherol peak area.
A.3.3.2 Determination of mixed tocopherols concentrate content
Total tocopherol content
msample2 Aint2
wref
??int1
Relevant content of d-??-tocopherol:
A??, ??4 -- ??- and ??-tocopherol peak area;
A??4 -- ??-tocopherol peak area.
A.3.3.3 Determination of the content of d-??-tocopheryl acetate and d-??-
tocopheryl acetate concentrate
A.3.3.3.1 Solution preparation
The internal standard solution is the same as A.3.3.1.1.
Reference solution: weigh 15 mg of d-??-tocopherol reference substance; accurate to
0.02 mg; place it in a brown volumetric flask; add internal standard solution dilute to
10.0 mL; cover the cork closely; shake to dissolve, then it?€?s done.
Sample solution: weigh an appropriate amount of sample; accurate to 0.02 mg; place
it in a brown volumetric flask; add internal standard solution to dilute to 10.0 mL; shake
to dissolve to gain a solution containing about d-??-tocopheryl acetate of 1.5 mg/mL.
A.3.3.3.2 Reference chromatographic conditions
SE-30 capillary column; hydrogen flame ion detector; keep the oven temperature at
250??C; the vaporization temperature and detection temperature are 300??C. The carrier
gas is nitrogen; adjust the carrier gas flow rate to make the internal standard peak
retention time at 18 min ~ 20 min. Inject 1 ??L of the reference solution into the
chromatograph; record the chromatogram. The theoretical plate number should be
larger than 1 500 according to the ??-tocopheryl acetate peak; repeat the injections;
the relative standard deviation of the correction factor should be no larger than 2.0%.
Inject 1 ??L of the sample solution into the chromatograph; record the chromatogram.
Make the relative retention time of the internal standard peak at 1.0, and the relative
retention time of the ??-tocopheryl acetate peak is about 0.6.
A.3.3.3.3 Correction factor determination
Inject 1 ??L of reference solution into the gas chromatograph; record the chromatogram;
measure Aref6, the peak area of the ??-tocopheryl acetate peak, and Aint6, the internal
standard peak area; calculate the correction factor f6 according to Formula (A.6)
Where:
Aint6 -- internal standard peak area;
Aint6
mref6
Aref6 ??int6
Sample solution: weigh 15 g of sample; accurate to 0.02 mg; place it in a brown
volumetric flask; add internal standard solution to dilute to 10.0 mL; shake to dissolve
to gain the solution.
A.3.3.4.2 Reference chromatographic conditions
SE-30 capillary column; hydrogen flame ion detector; keep the oven temperature at
250??C; the vaporization temperature and detection temperature are 300??C. The carrier
gas is nitrogen; adjust the carrier gas flow rate to make the internal standard peak
retention time at 18 min ~ 20 min. Inject 1 ??L of the reference solution into the
chromatograph; record the chromatogram. The theoretical plate number should be
larger than 1 500 according to the ??-tocopheryl acid succinate peak; repeat the
injections; the relative standard deviation of the correction factor should be no larger
than 2.0%. Inject 1 ??L of the sample solution into the chromatograph; record the
chromatogram. Make the relative retention time of the internal standard peak at 1.0,
and the relative retention time of the ??-tocopheryl acid succinate peak is about 0.6.
A.3.3.4.3 Correction factor determination
Inject 1 ??L of reference solution into the gas chromatograph; record the chromatogram;
measure Aref8, the peak area of the ??-tocopheryl acid succinate, and Aint8, the peak
area of the internal standard peak; calculate the correction factor f8 according to
Formula (A.8):
Where:
Aint8 -- internal standard peak area;
???????????? -- the concentration of ??-tocopheryl acid succinate reference substance, in
milligrams per milliliter (mg/mL);
Aref8 -- ??-tocopheryl acid succinate peak area;
??int8 -- internal standard solution concentration, in milligrams per milliliter (mg/mL).
A.3.3.4.4 Determination
Aint8
mref8
??int8 Aref8
keep for 30 s without fading; record the volume of the sodium hydroxide standard
titration solution.
A.5 Specific rotation
A.5.1 Reagents and materials
A.5.1.1 Anhydrous sodium sulfate.
A.5.1.2 Isooctane.
A.5.1.3 Potassium hydroxide.
A.5.1.4 Hydrochloric acid.
A.5.1.5 Sodium hydroxide solution: weigh 1 g of sodium hydroxide; use water to
dissolve; add water to dilute to 125 mL.
A.5.1.6 Sodium hydroxide solution containing 10% of potassium ferricyanide: take
10.0 g of potassium ferricyanide; add sodium hydroxide solution (1 ??? 125); shake to
dissolve; dilute to 100 mL;
A.5.1.7 Ethyl sulfate solution 1: Mix concentrated sulfuric acid and ethanol at a volume
ratio of 1:6.
2: Mix 1 mol/L of sulfuric acid and ethanol at a volume
ratio of 1:71.
A.5.2 Instruments and apparatuses
Use the instrument device specified in GB/T 613.
A.5.3 Analysis steps
A.5.3.1 d-??-tocopherol, mixed tocopherols concentrate
Weigh an appropriate amount of sample (equivalent to about 400 mg of tocopherol in
total); accurate to 0.2 mg; set in a separating funnel; use 50 mL of ether to dissolve;
add 50 mL of sodium hydroxide solution containing 10% of potassium ferricyanide;
shake for 3 min; use water to wash the ether solution for four times, with 50 mL of
water each time. Use anhydrous sodium sulfate to dry the ether solution; place the
dried diethyl ether solution in a water bath to reduce pressure or under the nitrogen at
atmospheric pressure to evaporate and concentrate to about 7 mL ~ 8 mL; then stop
heating; let the ether evaporate to dryness. Use 25.0 mL of isooctane to dissolve the
residue immediately; at 25??C ?? 0.5??C, use the method specified in GB/T 613 to
measure the optical rotation; and calculate the specific rotation according to Formula
(A.10).
A.5.3.3 d-??-tocopheryl acid succinate
Weigh an appropriate amount of sample (equivalent to about 400 mg of ??-tocopherol);
accurate to 0.2 mg; place in a 250 mL round bottom flask; add 50 mL of absolute
ethanol to dissolve; reflux for 1 min; when the solution is boiled, slowly add 1 g of
granular potassium hydroxide from the condenser; avoid overheating; continue to
reflux for 20 min; add 2 mL of hydrochloric acid through the condenser; let it cool;
transfer the solution to a 500 mL separating funnel; use 100 mL of water and 100 mL
of diethyl ether to wash the flask; place the washing solution in a separating funnel;
shake vigorously; put it aside for layering; for the aqueous layer, use diethyl ether to
extract twice, 50 mL each time; combine the ether extracts; then use water to wash for
4 times, 100 mL each time; place the ether solution in a water bath to reduce pressure
or under a nitrogen stream to concentrate the volume to about 7 mL ~ 8 mL; then stop
heating; continue to evaporate ether to dryness; immediately add 220 mL of ethyl
sulfate solution to dissolve the residue; transfer to a separating funnel; use a small
amount of ethyl sulfate solution to wash the container twice; then transfer to the
separating funnel; add 200 mL of water; use diethyl ether to extract, for 3 times, for 75
mL the first time, and 25 mL the second and the third times respectively; combine the
ether solutions; add 50 mL of sodium hydroxide solution containing 10% of potassium
ferricyanide; shake for 3 min; carry out the following procedure in the same manner as
in A.5.3.1. Calculate the specific rotation according to Formula (A.12).
Where:
?? -- the measured optical rotation;
L -- length of the measuring tube, in decimeters (dm);
X -- content of tocopheryl acid succinate in the sample, %;
m -- sample quality, in grams (g);
-- concentration of the measuring solution, in grams per milliliter (g/mL);
0.811 -- unit conversion index relative to d-??-tocopherol.
A.6 Determination of absorbance coefficient
A.6.1 Reagents and materials
Absolute ethanol.