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GB 1903.20-2016: (Food safety national standard food nutrition enhancers -- Thiamine nitrate)
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(Food safety national standard food nutrition enhancers -- Thiamine nitrate)
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GB 1903.20-2016
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Basic data | Standard ID | GB 1903.20-2016 (GB1903.20-2016) | | Description (Translated English) | (Food safety national standard food nutrition enhancers -- Thiamine nitrate) | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Word Count Estimation | 7,770 | | Date of Issue | 2016-12-23 | | Date of Implementation | 2017-06-23 | | Regulation (derived from) | National Health and Family Planning Commission Notice No.17 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | GB 1903.20-2016: (Food safety national standard food nutrition enhancers -- Thiamine nitrate)---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 safety national standard food nutrition enhancers thiamine nitrate)
National Standards of People's Republic of China
National Food Safety Standard
Fortified Food thiamine nitrate
Published 2016-12-23
2017-06-23 implementation
National Health and Family Planning Commission People's Republic of China
China Food and Drug Administration issued
National Food Safety Standard
Fortified Food thiamine nitrate
1 Scope
This standard applies to acrylonitrile or the like as a main raw material malononitrile food fortifier by chemical synthesis of thiamine nitrate.
2 Chemical name, molecular formula, structural formula and relative molecular mass
2.1 Chemical Name
4-methyl-3 - [(2-methyl-4-amino-5-pyrimidinyl) methyl] -5- (2-hydroxyethyl) thiazole nitrate bromide
Formula 2.2
C12H17N5O4S
2.3 formula
2.4 Molecular Weight
327.37 (according to 2013 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall comply with the requirements in Table 1.
Table 1 Sensory requirements
Project requires test methods
White or white color
Odor odorless or slight specific odor
State of powder or crystalline powder
Take about 2g sample is placed in a clean, dry white dish, under natural light,
Observe the color and state, smell the smell
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
Thiamine nitrate (C12H17N5O4S, dry basis) content, w /% ≥ 98.0 Appendix A A.4
pH (20g/L) 6.0 ~ 7.5 GB/T 23769
Loss on drying, w /% ≤ 1.0 A.5 Appendix A
Residue on ignition, w /% ≤ 0.1 A.6 Appendix A
Chloride (based on Cl), w /% ≤ 0.06 A.7 Appendix A
Sulfate (in terms of SO4), w /% ≤ 0.011 A.8 Appendix A
Lead (Pb)/(mg/kg) ≤ 1.0 GB 5009.12
Total arsenic (As)/(mg/kg) ≤ 1.0 GB 5009.11
Appendix A
Testing method
A.1 Safety Tips
Reagents of this standard test methods used toxic or corrosive, operating according to the relevant regulations, required careful operation. If splash
To the skin immediately wash with water, severe cases should be treated immediately. , Be carried out in a fume hood when using a volatile acid.
A.2 General Provisions
The reagents used in this standard, unless otherwise specified, only confirmed in the analysis of analytical grade reagents and GB/T 6682 in a predetermined three
water. Standard Solution, product formulation and testing methods required, in the absence of other requirements specified, are by GB/T 601, GB/T 603
Preparation of regulations.
A.3 Identification Test
A.3.1 solubility test
Slightly soluble in water, slightly soluble in methanol.
A.3.2 color ferrous sulfate
A.3.2.1 Reagents and materials
A.3.2.1.1 sulfuric acid.
A.3.2.1.2 ferrous sulfate solution. Take 8g ferrous sulfate (FeSO4 · 7H2O), was added 100mL boiling over cold water and dissolved, shake,
Using now.
Procedure A.3.2.2
Take a sample of approximately 10mg, test tube, add water to dissolve 1mL, the same amount of sulfuric acid, mixed and allowed to cool, dissolved ferrous sulfate was added along the wall
Liquid, so that liquid into two layers, then the interface was brown liquid.
A.3.3 chromogenic lead acetate
A.3.3.1 Reagents and materials
A.3.3.1.1 lead acetate.
A.3.3.1.2 lead acetate solution. Take lead acetate 10g, add boiling over cold water was dissolved, the solution was added dropwise acetic clarified, plus boiling over cold
Water volume to 100mL, that is, too.
A.3.3.1.3 sodium hydroxide solution. 100g/L.
Procedure A.3.3.2
Sample taken about 5mg, which was dissolved in a mixed solution of a solution of lead acetate and 1mL 1mL sodium hydroxide solution, the solution was yellow, water bath
The mixed solution was heated for several minutes, the solution turned brown, black precipitate on standing due.
A.3.4 Fluorescence
A.3.4.1 Reagents and materials
A.3.4.1.1 sodium hydroxide solution. 40g/L.
A.3.4.1.2 potassium ferricyanide solution. 100g/L.
A.3.4.1.3 hydrochloric acid solution. 36.5g/L.
A.3.4.1.4 n-butanol.
Procedure A.3.4.2
Sample taken about 5mg, after adding sodium hydroxide solution to dissolve 2.5mL, 0.5mL was added potassium ferricyanide solution and 5mL n-butanol, Qiang Lie
Shaking 2min, placed allowed to separate, the upper layer was a strong blue fluorescence. After about 1mL hydrochloric acid solution was added, the fluorescence disappeared; then about
After 3mL of sodium hydroxide solution, and show fluorescence.
A.4 Determination of thiamine nitrate (C12H17N5O4S, dry basis) content
A.4.1 Reagents and materials
A.4.1.1 anhydrous formic acid.
A.4.1.2 acetic anhydride.
A.4.1.3 perchloric acid standard titration solution. c (HClO4) = 0.1mol/L.
A.4.2 Analysis step
Weigh about 0.14g sample, accurate to 0.0001g, placed in a conical flask, add anhydrous formic acid dissolved 5mL, 70mL acetic anhydride was added,
According to potentiometric titration, the titration standard solution was titrated with perchloric acid, and titration with blank correction.
A.4.3 calculation results
Thiamine nitrate (C12H17N5O4S, dry basis) content of the mass fraction w1, calculated according to formula (A.1).
w1 =
(V-V0) × c × M
m × (1-w2) × 1000 ×
100% (A.1)
Where.
V --- standard sample consumption perchloric acid titration solution volume in milliliters (mL);
--- consumption volume V0 blank perchloric acid standard titration solution in milliliters (mL);
The actual concentration of standard C --- perchloric acid titration solution in units of moles per liter (mol/L);
--- M thiamine nitrate (
2C12H17N5O4S
) Molar mass in grams per mole (g/mol) [M (
2C12H17N5O4S
= 163.7g/mol];
--- m sample mass in grams (G);
w2 --- A.5 measured by loss on drying,%;
1000 --- conversion factor.
The arithmetic average of the measurement results parallel the measurement results, the measurement results of two parallel allows absolute difference not more than 0.3%.
Determination of loss on drying A.5
A.5.1 Analysis step
Weigh about 1g sample, accurate to 0.0001g, was placed on the dried to constant weight weighing bottle 105 ℃ ± 2 ℃, at 105 ℃ ± 2 ℃
Oven dried to constant weight.
A.5.2 calculation results
Loss on drying mass fraction w2, calculated according to equation (A.2).
w2 =
m1-m2
m × 100%
(A.2)
Where.
The total mass of the sample before drying and M1 --- weighing bottles in grams (G);
--- M2 After drying and weighing the total mass of the sample bottles in grams (G);
--- m sample mass, in grams (g).
The arithmetic average of the measurement results parallel the measurement results, the measurement results of two parallel allows the absolute difference is not greater than 0.1%.
Determination of residue on ignition A.6
A.6.1 Analysis step
Weigh about 1g sample, accurate to 0.0001g, was placed on ignition to constant weight in a porcelain crucible at 750 ℃ ± 50 ℃, low heat and slowly add
Heat to completely carbonized, After cooling, add 0.5mL of sulfuric acid from about the sample to completely wet, and heated to a low temperature after the sulfuric acid vapor divisible, into a high temperature furnace
In to burning at 750 ℃ ± 50 ℃ constant weight.
A.6.2 calculation results
Ignition residue content of w3, calculated according to formula (A.3).
w3 =
m3-m4
m × 100%
(A.3)
Where.
--- M3 total mass of the crucible and the residue, in grams (G);
--- M4 crucible mass in grams (G);
--- m sample mass, in grams (g).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to 0.02%.
Determination A.7 Chloride (Cl) of
A.7.1 Reagents and materials
A.7.1.1 nitric acid solution. 10% (volume ratio).
A.7.1.2 silver nitrate solution. c (AgNO3) = 0.1mol/L.
Chloride standard solution A.7.1.3 Ⅰ. chlorine 0.1g/L. Take 0.165g of sodium chloride in 1000mL volumetric flask, dissolved in water and diluted to
Scale.
Chloride standard solution A.7.1.4 Ⅱ. chlorine 0.01g/L. Ⅰ10mL suction chloride standard solution in 100mL volumetric flask, dilute with water
Release to the mark.
A.7.2 Analysis step
A sample was weighed 0.10g, set 50mL Nessler tube, dissolved in water, to make into a 25mL, 10mL and dilute nitric acid, adding water to about
40mL, shake, as the test solution; 6.0mL take Ⅱ chloride standard solution, set another 50mL Nessler tube, in the same manner so that
Into 40mL, shake, as the control solution; 1.0mL were added to two of the silver nitrate solution, diluted with water to 50mL, shake, in the dark
Turbidity is placed at 5min, on a black background with the set, viewed from the direction of color than the tube, comparing the turbidity of the test solution can not be compared with the control solution
The degree of concentration.
Determination A.8 Sulfate (SO4 basis)
A.8.1 Reagents and materials
Hydrochloric acid solution A.8.1.1. take 23.6mL hydrochloric acid, diluted with water to 100mL.
Sulfuric acid solution A.8.1.2. c [
(H2SO4)] = 0.01mol/L.
Barium chloride solution A.8.1.3. c (BaCl2) = 0.5mol/L.
A.8.1.4 stoppered cuvette. 50mL.
A.8.2 Analysis step
1.5 g sample was weighed (accurate to 0.01g) in 50mL colorimetric tube with a stopper, add about 30mL of water and 2mL dilute hydrochloric acid solution to dissolve,
Diluted with water to 50mL, prepare a sample tube. Take another branch 50mL stoppered cuvette, was added 0.35mL of sulfuric acid solution and 2mL dilute hydrochloric acid
Solution, diluted with water to 50mL, prepared by standard tube. To the two cuvettes 2mL barium chloride solution were added, mixed, allowed to stand
10min, a black background transverse turbidimetric visual, not white of the sample tube is deeper than the standard tube.
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