Some standard content:
All technical contents of this standard are mandatory. This standard corresponds to the d-tocopherol concentrate (d-Tacophetol Coureatrale), tosopherols concentrate (Mixed), d-treophcrvlArulale>, di-tuvpheryl acetate concentrate (du-tuvphery acetic acid concentrate), d-t-butyl acetic acid concentrate (d-t-butyl acetic acid concentrate), d-t-butyl acetic acid concentrate (d-t-butyl acetic acid concentrate), etc. The degree of non-equivalence is not equivalent. Among them, the content index of tl-t-butyl acetic acid is higher than that of Appendix A of CCFV-1996. This standard was drafted by: Jiangjiang Pharmaceutical Co., Ltd., Zhejiang Haizhi Pharmaceutical Co., Ltd. The main drafters of this standard are: Ping Xiaole, Zhengqin Biao, Pian Kaiming, Qian Meng, Gan Jiaqiu, Qian Liujian, Gong Gan. 1 Scope
Food Additive Natural Vitamin E
GB19191-2003
This standard specifies the scope, requirements, test method, inspection rules, labeling, etc. of food additives natural vitamin E, packaging, transportation and storage
This standard is applicable to products with a low content of natural vitamin E in edible foods and prepared with edible oils. d-α-Tocopherol is suitable for use as a nutritional and antioxidant agent in the food industry; d-acetic acid tocopherol, d-acetic acid phenol concentrate, and α-tocopherol phenol are suitable for use as nutritional and antioxidant agents. 2 Normative references || tt || The clauses in the following documents become the clauses of this standard through reference in this standard. For any referenced document with a date, all subsequent static copies (excluding those indicating errata) or versions shall not be applicable to this standard. However, the latest versions of these documents may be used by the parties who have reached an agreement based on this standard. For any referenced document without a date, the latest version shall apply to the standard. GB/T601 Preparation of standard titration solutions for chemical reagents GB/T602 Preparation of standard solutions for determination of chemical reagents (GB/T502-2002.net S() G351-1:19A2) GR/T613 General method for comparative photometric determination of chemical reagents (G/T613-1988.1 G16E3-1:1982) GF/T84:1 Test method for limits of heavy metals in food additives (Chinese Pharmacopoeia, 2003 edition, Part II, 3 Classification and nomenclature) .1 Classification
Food vitamin E can be divided into d-vitamin E concentrated wax, phenol extract, α-tocopherol, α-tocopherol concentrate, d-tocopherol products, and its 10+ tocopherol secretion liquid is divided into FC type and 7O type. 3.2 Product name
This product has four homologues according to the different substituents and phase differences, including d-tocopherol, d-tocopherol, dY-tocopherol and d-tocopherol and the corresponding esters and monoesters. It should be d-\-tocopherol, d-aldehyde or d-a-aldehyde. Chemical name
da phenol: 51>2.5.7,8-tetramethyl-2-(4.8.12-7-methyl-1-decyl)-6-pyrrol-1-ol dα-acyl ester: 1+) 2,5.7.8-tetramethyl-2-(4.8,12-1-decyl)-6-chromanol-6-acetic acid 2-0-acetic acid: (10) 2,2.7.R-trimethyl-2-(1.3,12-trimethyl-1-trialkyl)chromanol 1-ol 2-ol 3-ol Molecular formula
dl--CHO
da acetic acid: LaHO
da-1-ol phenol: CH
3.4 Relative molecular weight
d--biomass ratio 43.7 calculated according to 1 year relative atomic mass ratio -a-aldehyde acid 472.5 (according to 1595 international relative atomic mass ratio) 2x total molecular weight 550.79 (according to 1999 international relative atomic mass ratio) 1
GB19191-2003
3.5 Structural formula
R, .- is the relative molecular weight
R, CH,CO- is the relative molecular weight hydroxyapatite
KHCHOCHC is the relative molecular weight
4.1 Properties
Cha,t: (HC(C,, c)
himself. The raw phenol is burned in a red clear liquid, which is very urgent. It is oxidized by light and air, and the color of the new raw material is dark red to yellow. It is allowed to float and exchange with the oil filter. It has special odor and taste, light or air sensitivity. It slowly hydrogenates and the color gradually becomes darker (more special in the finished product). Tocopherol--Vinegar is a colorless to clear copper-colored liquid micro-body, almost no effect, it may solidify, and it is unstable in the test medium after 25 hours of baking:
HD-Vinegar raw phenol is concentrated into a light brown viscous condensate, which is almost unstable in the test medium: - Cyclopentanol is white The product is white powder, almost inert and tasteless, and is not affected by air, alkali or heat, and melts at about 75°C.
This product is not soluble in water, but is easily decomposed in water and ethanol. It is easily dissolved in water, ethanol, and plants: 4.2 Physical and chemical indicators
The physical and chemical indicators of the product additive natural vitamin E are in accordance with the provisions of Table 1.
Table 1 Physical and chemical indicators of the product additive natural vitamin E refer to
Total dust (in 1h liter>/tmg/kg)
d-type growth
components
northeast dragon love [
components (in 1h liter>/tmg/kg)
do-main medical concentration range
7*53. 3 2*70.0
very suitable for growth
acid condensation
3 1 20-
65.3--132.
da-in addition to the three
growth gradually concentrated
· 24
C-building amber resistance to growth
35.6--102.
8.c.-.15.3
Note that the content can be expressed in the same year (/, 1-growth type-1.V.1-late growth-1.36.1 our acid content-1,1,
5 test method
GD 19191—2003
Unless otherwise specified, all reagents used in the test are analytically pure reagents. The water shall comply with the provisions of purified water in the 20th edition of the Pharmacopoeia (Part I). The water shall comply with the provisions of GB/T601, 6R/TC2, and 2003 editions of the Pharmacopoeia. The instruments and equipment are the same as those generally used in practice.bZxz.net
Note: The content and specific radiation test shall be carried out separately. The test shall be kept away from light. 5.1 Identification
5.1.1 Reagents and materials
a) Light water;
b) Nitrate.
5.1.2 Identification method
5.1.2.1 Take about 50 mg of the test sample and add 10 ml of anhydrous 7-ethanol to dissolve it. Add 7 ml of nitric acid and heat at 75°C for 5 minutes until it turns from light red to orange.
5.1.2.2 On the gas chromatogram of content determination, the main peak of the test sample (the second main peak for the test sample) and the main peak of the reference sample should be consistent in time (except for the peak of the test sample and the internal standard peak). 5.2 Content determination
The determination shall be carried out according to the method in Appendix A. The allowable error shall be the arithmetic mean of the results obtained by two parallel determinations. The deviation of the results of two parallel determinations shall not be greater than 2.0% for d-tocopherol concentrate and mixed tocopherol concentrate, and not greater than 1.5 for α-tocopherol acetate, d-α-hydroxytocopherol concentrate and dn-tocopherol.
5.3.1 Reagents and materials
a) Ether:
bl anhydrous ethanol;
r) Hydroxide standard solution titration rate (0.1mol/L) d) Indicator (→10)
5.3.2 Determination
Measure 15mL of anhydrous ethanol and ether, place in a flask, add enzyme acid indicator U.=mL, dropwise add sodium hydroxide standard solution to titrate until slightly pink, add more than 1.0% test solution, titrate until the solution is pink, and the color does not change after 305. The volume of the standard solution of sodium hydroxide is determined by the consumption of oxygen. 5.4 Comparison
5. 4. 1 Instruments
Use the instruments specified in G/TS1,
5.4.2 Reagents and materials
a) Anhydrous sodium hydroxide:
6 isooctane
Potassium hydroxide:
Salt:
Hydrogen oxidized solution (1-→125);
10% potassium ferric chloride molten: potassium ferric chloride 10.0R. Add oxygen to oxidize solution (1→12G> Make the solution to 100ml
Add ether and ethanol drops (1--7), take 1 part of concentrated sulfuric acid solution and add 7 parts of ethanol, mix well to get. (1→72), take 1 part of vegetable acid bath and add 72 parts of 7. alcohol, mix to get 3
GBt9191203
5.4. 3.1 Da-tocopherol concentrated solution. Weigh an appropriate amount of the combined tocopherol concentrate sample (about 400g of total tocopherols) and add 53ml of ethyl acetate [the core of the product is sodium fluoride and potassium fluoride solution] 1. Wash the filtered solution with water for 3 minutes, each time with 5ml of water. Take acetic acid solution and add water to make it cool. After burning acetic acid for a while, evaporate it in nitrogen gas in a small container. When it is about 7mL~8mL, stop heating and continue to dissolve it in a jar. Add 25.0mL of acetic acid immediately and stir at 251C.5℃ to determine the luminous intensity according to the method specified in H2O. The luminous intensity is calculated by formula (1):
—1XxX25
;
—the length of the measuring tube, in decimeter (dm): —the mass of the test piece, in gram (g):
—the acetic acid content, %
m/25, the liquid concentration of the test piece is gram per ml (g/ml) 5. 4.3.2 d-rz-acetic acid, d-al-acetic acid concentrate.......( )
Take a sample (accurately equivalent to about 2-4g of commercially available bioremediation), heat it at 150°C and add 25% ethanol to make the solution decompose (→7). Transfer the cooled liquid into a separatory flask with a small amount of ethyl acetate (31→72). Select and filter, add 20mL of water, use 7 mL each time, 75mL for the first time and 25mL each time. 10% sodium hydroxide suspension 5umL, full %min below 5.4.1Wanda operation, 5.4.3.3dx-alumina acid ester
weigh into a suitable plate (drug equivalent to -101F accurate to 3.2mg), kidney 25T. purple bottle, anhydrous ethanol wmL solution: reflux 1min: when the liquid boils, add potassium hydroxide from the refrigerator: avoid overheating: continue to reflux 21min, drip 2mL of acid through the condenser, transfer the cold liquid to 5u0ml of boiling water, 100ml of water. Acetaldehyde 1CC m. Boil the cake and wash it in a separatory funnel, stir vigorously, and separate the layers after static stratification. Extract 3 times with water: collect the ethanol at each stage, and cool it down to 400 mL. When the volume is reduced to 7 mL, stop heating and continue to separate the ethanol. Draw a clear line and dissolve the ethanol at 2°C. Transfer the liquid to the separatory funnel with a small amount of ethanol (1→7%) and transfer it into a separatory funnel. Add 2 L of water, press 3% ethanol, and mix the ethanol solution for the first and second times. Add 1 mL of 2% ethanol. Potassium hydrogen record the cost of dripping liquid m1. Recommended 3min below the same as 5.4.3.1 visit operation,
5.5 heavy metal
Take this product \k burnt snail. According to GH/D 8451 ten method digestion method. 6 Inspection rules
6.1 This product, after the final combination of ear homogeneous finished product is a batch. 6.2 sampling, block packaging is pieces, for the ear batch total pieces, total pieces 3, each piece collection: 2300 monthly collection number according to 1 draw total effect 200, sampling number // 11, the same time push collection sample. And after equal plate limit size collection of 10 times the test amount, divided into two prices packed in clean ten dry 6.3: This product needs to be inspected by the inspection department of the production unit according to the standard. The production unit guarantees that the products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality acceptance certificate. 5.4: The unit can carry out quality control and inspection on the received products according to the inspection plan and test methods specified in this standard to see if their indicators meet the requirements specified in this standard. 191912003
6.5 If one of the indicators in the blood test does not meet the requirements of this standard, a new sample should be taken from the packaging of the two batches, and the unqualified batch should be inspected again. If the inspection result is still unqualified, the batch is judged as unqualified. 7 Labels and signs
The product packaging should have obvious and firm signs or labels, and indicate the food additives. The content should include: manufacturer name, factory name, product name, product pass number, batch or production date, shelf life, net weight, product standard, production license, and unit (unit) quantity
8 Packaging, transportation and storage
8.1 Packaging
This product should be packed in aluminum containers that meet the food production requirements, and stored in a nitrogen-tight container to prevent damage and heat. The quantity deviation should meet the relevant regulations of the environment: the packaging specifications can be determined according to the requirements of the user's manual. The packaging should meet the transportation and storage requirements. 8.2 Transportation
This product should not be packed or shipped together with toxic, toxic, or other polluting substances and oxidizing substances. It should be kept away from dust, rain, noise and pollution.
8.3 Storage
This product should be stored in a dry place under the shade of the sun. 8.4 Shelf life
Under the storage conditions specified in the standards and the packaging is intact and the seal is not opened, the shelf life is 13 years: open and use immediately.
GD 19191—2003
t. 1 Reagents
1.1 Tocopherol-F-hexadecene
Color analysis,
A.1.2 (-tocopherol reference substance
Should meet the following requirements:
Appendix A
(Normative record)
Content determination
Properties: Slightly yellow to off-white icy liquid, containing 95.0%
A.1.3 r-tocopherol acetate reference substance
Should meet the following requirements:
Properties: Slightly yellow to yellow viscous oily liquid:
Content%
A.1.4 α-tocopherol acetate reference substance
Should meet the following requirements;
Properties: Special package to color, containing 58. 3%.
A.1.5 n-hexane
A.2 Receiver
Gas phase chromatography.
A,3 Determination
According to the gas phase chromatography method in the appendix of the Pharmacopoeia of the People's Republic of China, Volume 3, 2002. A.3,1-(-) ... Weigh an appropriate amount of sample, accurate to 0.02m/s, add the internal standard and dilute to 1.m/s, shake to dissolve, and obtain the corrected sample at 1.5 /mL was dispersed. A.3.1.2 Chromatographic conditions
SF-3-tube chromatograph, hydrogen ion detector, column density 250, vaporization temperature and humidity 00: store as commercial gas, avoid the entire carrier gas flow and keep the time between 12mn and 2min. Pipette 1 L of reference solution, let it fall into the instrument, record the chromatogram, write the number of peaks according to the growth rate should be greater than 1: repeat the injection multiple times, the relative error of the calibration factor should not be greater than 2. Divide, change the test sample to 1 drop chain, let the doctor record the spectrum, the relative retention time of the original internal standard is about 1.0, the relative retention time of the peak of β- and 7- is about 0.8, and the relative retention time of the peak of B- is about 1.0. The relative retention time of ethanol is about 0.A.3.1.3 Correction factor determination
Gll19191—2003
Take the sample solution for gas chromatography and record the negative spectrum: single sample peak area rent internal standard peak call surface A calculated and corrected by formula (A.1):
A person na:/10
In the formula,
·Correction factor
Internal standard sample area,
[. Internal [a
|positive ethanol peak trend and surface rent! :
Internal standard soluble substance unit is gram per liter (mg/ml) paired sample limit time tolerance reference substance dosage, unit () 1. 3. 1.4 Determination
Long supply finished product liquid 1 positive generation sweep color fall discussion. Record the chromatogram, (calculate -lanyupan and Shengxiaonai, 8-lanyan peak bee area AAA:! And calculate the effect of the previous item (A) and the internal drop area to calculate the content rate by formula (A.2) formula 3: A. &. G
Total organic matter content: X
ATXw/1C
Relative content of small-u-fertility compound: X. In the formula,
Total organic matter content!
d-0-organic matter content:
Calibration,
Original organic matter peak point and peak area:
Internal standard net surface area
α-phenol peak surface area,
Internal standard liquid concentration is g/ml (gL ), x1%
Prepare the actual product solution for the product, the unit is g (! A.3.2 Mixed tocopherol solution
A.3.2.1 Prepare the internal standard solution, the same as A.3.1.1A2
Test sample: Take the sample and add it to the standard solution until it reaches u.2m, add the internal standard solution to dilute it, and then get the drug containing 3-10:d-tocopherol 1.5:rtL. A.3.2.2 Chromatographic conditions
Same as A 5. 1. 2.
A.3.2.3 Calibration chart determination
Company 4.5. 3.
A. 3. 2. 4 Drama
Results of the trial product fell with 1L legal person one color treatment only, record the color language reason calculation α-birth sound age production and fertility price, 3-birth green long final light area: 4A1.). Calculate the previous item A and the internal standard body single industry within the support (A,) formula (A, calculation signature including profit: *: XX×10g
Benefit heart--fertility--Lan:
Am-Am×100%
(B19 191—2003
X--—Total fertility drug containing positive;
.? fertility
0-tocopherol reference substance amount:
correction factor,
tocopherol peak total library area:
internal standard peak blood volume;
tocopherol peak area;
tocopherol peak call area:
internal standard drop concentration, the unit is grams per liter
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