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GB 1886.75-2016: National Food Safety Standard -- Food Additives -- L-Cysteine Hydrochloride
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National Food Safety Standard -- Food Additives -- L-Cysteine Hydrochloride
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GB 1886.75-2016
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Basic data | Standard ID | GB 1886.75-2016 (GB1886.75-2016) | | Description (Translated English) | National Food Safety Standard -- Food Additives -- L-Cysteine Hydrochloride | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Word Count Estimation | 24,282 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-01-01 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | GB 1886.75-2016: National Food Safety Standard -- Food Additives -- L-Cysteine Hydrochloride---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 additive - L-cysteine hydrochloride)
National Standards of People's Republic of China
National standards for food safety
Food Additives L-Cysteine Hydrochloride
2016-08-31 released
2017-01-01 Implementation
People's Republic of China
National Health and Family Planning Commission released
National standards for food safety
Food Additives L-Cysteine Hydrochloride
1 Scope
This standard applies to livestock and poultry hair, feathers as raw materials by hydrolysis, or starch as raw material by Escherichia coli Escherichia coli K-12
The food additive L-cysteine hydrochloride.
2 chemical name, molecular formula, structural formula and relative molecular mass
2.1 Chemical name
L-2-amino-3-mercaptopropionate monohydrate
L-2-amino-3-mercaptopropionate hydrochloride
2.2 Molecular formula
C3H7NO2S · HCl · H2O
C3H7NO2S · HCl
2.3 Structural formula
2.3.1 L-cysteine hydrochloride monohydrate
2.3.2 L-cysteine hydrochloride Anhydrous
2.4 Relative molecular mass
175.64 A water (according to.2007 International relative atomic mass)
157.62 Anhydrous (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
The project requires a test method
Color white
State crystalline or crystalline powder
Take the appropriate amount of sample in a clean, dry white porcelain dish
Natural light, observe the color and state
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
project
index
Water-free
Testing method
L-cysteine hydrochloride content (on a dry basis), w /% 98.5 to 101.0 98.0 to 102.0 Appendix A, A.3
Specific rotation αm (20 ℃, D)/[(°) · dm2/kg] 5.5 ~ 7.0 5.6 ~ 8.9 Appendix A A.4
pH 1.5 to 2.0 1.5 to 2.0 Appendix A, A.5
Chloride (in Cl), w /% 19.8 to 20.8 22.3 to 22.6 Appendix A, A.6
Dry reduction, w /% 8.0 ~ 12.0 ≤ 2.0 Appendix A A.7
Residue on ignition, w /% ≤ 0.10 0.10 Appendix A, A.8
Transmittance, w /% ≥ 98.0 98.0 Appendix A A.9
Sulfate (calculated as SO4), w /% ≤ 0.03 0.03 Appendix A. A.10
Ammonium salt (calculated as NH4), w /% ≤ 0.02 0.02 Appendix A A.11
Other amino acids, w /% ≤ 0.5 0.5 Appendix A. A.12
Iron salt (in terms of Fe)/(mg/kg) ≤ 10.0 10.0 Appendix A A.13
Heavy metals (Pb)/(mg/kg) ≤ 10 10 Appendix A A.14
Arsenic (As)/(mg/kg) ≤ 1.0 1.0 Appendix A A.15
Appendix A
Testing method
A.1 General provisions
The reagents and water used in this standard, when not specified in other requirements, refer to the analysis of pure reagents and GB/T 6682 provides three levels of water. test
The standard solution, impurity standard solution, preparation and preparation used in the test shall be classified according to GB/T 601, GB/T 602 and
GB/T 603. The solution used in the test refers to the aqueous solution when it is not specified in the formulation of the solvent.
A.2 Identification test
Weigh the sample about 1mg, add about 120mg of potassium bromide, grinding evenly, tablet, recording the infrared spectrum of the sample should be with the L-cysteine
The standard infrared spectra of the hydrochloride monohydrate are consistent, see Appendix B.
A.3 Determination of L-cysteine hydrochloride content (on a dry basis)
A.3.1 Methodological Summary
Oxidation of the test sample with iodine as oxidant, and titration of the remaining iodine with sodium thiosulfate standard solution, indirect calculation of the oxidation sample
The amount of iodine consumed, according to the amount of iodine consumed by the oxidation sample, and finally calculate the sample content.
A.3.2 Reagents and materials
A.3.2.1 Hydrochloric acid solution. 10%.
A.3.2.2 Sodium thiosulfate standard titration solution. 0.1 mol/L.
A.3.2.3 iodine standard titration solution. 0.05 mol/L.
A.3.2.4 Starch indicator. 10 g/L.
A.3.3 Analysis steps
Weigh the sample about 0.25g, accurate to 0.0001g, add water 20mL and potassium iodide 4g, shaking dissolved, add hydrochloric acid solution 5mL,
Fat belly suction tube by adding iodine standard titration solution 25mL, placed in the dark for 15min, and then placed in an ice bath for 5min, with sodium thiosulfate standard
Quasi titration solution titration, near the end point, add starch indicator solution 2mL, continue to titrate to solution blue disappears. At the same time do blank test.
A.3.4 Calculation of results
The mass fraction w1 of the L-cysteine hydrochloride content (on a dry basis) is calculated according to the formula (A.1)
w1 =
c1 × (V1 - V2) × M
m1 × 1 - w2 () × 1000 ×
100% (A.1)
Where.
c1 --- sodium thiosulfate standard titration solution concentration, the unit is mol per liter (mol/L);
V1 --- blank consumption of sodium thiosulfate standard titration solution volume, in milliliters (mL);
V2 --- sample consumption of sodium thiosulfate standard titration solution volume, in milliliters (mL);
M-L-cysteine hydrochloride in moles per mole (g/mol), [M (C3H7NO2S · HCl) =
157.6];
m1 --- the quality of the sample, in grams (g);
w2 --- dry weight reduction of sample,%;
1000 --- conversion factor.
The results of the test are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
The value is not greater than 0.3%.
A.4 Determination of specific rotation αm (20 ° C, D)
A.4.1 Instruments and equipment
Polarimeter (accuracy ± 0.001 °). with sodium light (sodium spectrum D line 589.3nm) as a light source.
A.4.2 Reagents and materials
Hydrochloric acid solution. 1mol/L.
A.4.3 Analysis steps
Weigh the sample about 8g, accurate to 0.0001g, placed in 100mL volumetric flask, add 1mol/L hydrochloric acid solution dissolved, adjust the solution
Temperature to 20 ℃, diluted to the mark, shake. With a small amount of this liquid rinse the rotating tube several times, and then slowly into the liquid crystal tube (not to occur
Bubble), the rotating tube placed in the polarimeter detection.
A.4.4 Calculation of results
The specific rotation of the sample at 20 ° C on the D spectrum of the sodium spectrum αm (20 ° C, D) is calculated according to the formula (A.2)
αm (20 ° C, D) =
100 × α
l × c2
(A.2)
Where.
100 --- conversion factor;
α - optical rotator measured by the optical rotation, the unit is degrees (°);
l - the length of the rotating tube in dm (dm);
c2 --- 100mL solution contained in the quality of the measured substance (dry basis), in grams (g).
A.5 Determination of pH
Weigh the sample 0.20g, add water 20mL dissolved, measured with a pH meter. The results of two independent determinations obtained under reproducible conditions
The difference is not greater than 0.2.
A.6 Determination of chloride (in Cl)
A.6.1 Reagents and materials
A.6.1.1 nitrobenzene.
A.6.1.2 Hydrogen peroxide. 30%.
A.6.1.3 nitric acid solution. 50mL of nitric acid, diluted with water to 100mL, shake.
A.6.1.4 potassium permanganate solution. 0.01 mg/mL.
A.6.1.5 Silver nitrate standard titration solution. 0.1mol/L.
A.6.1.6 Ammonium thiocyanate standard titration solution. 0.1mol/L.
A.6.1.7 Ammonium Sulfate Indicator.
A.6.2 Analysis steps
Weigh the sample about 0.25g, accurate to 0.0001g, add 10mL water and 10mL nitric acid solution dissolved, with fat belly straw to add nitric acid
Silver standard titration solution 25mL and potassium permanganate solution 50mL, water bath for 30min, let cool, add hydrogen peroxide solution to solution into no
Color, then add ammonium sulfate indicator 8mL and nitrobenzene 1mL, with ammonium thiocyanate titration solution titration. At the same time do blank test.
A.6.3 Calculation of results
The mass fraction w3 of the chloride (in terms of Cl) is calculated according to formula (A.3)
w3 =
c3 × (V3 - V4) × M
m2 × 1000 ×
100% (A.3)
Where.
c3 - the concentration of ammonium thiocyanate standard titration solution in moles per liter (mol/L);
V3 --- blank consumption of ammonium thiocyanate standard titration solution volume, in milliliters (mL);
V4 --- sample consumption of ammonium thiocyanate standard titration solution volume, in milliliters (mL);
M - the molar mass of the chloride ion in grams per mole (g/mol), [M (Cl -) = 35.45];
m2 --- the quality of the sample, in grams (g);
1000 --- conversion factor.
The results of the test are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
The value is not greater than 0.1%.
A.7 Determination of dry reduction
A.7.1 Analysis steps
A.7.1.1 Place the weighing bottle in a vacuum oven, reduce it to less than 2.67 kPa at room temperature, weigh no more than 0.0003 g before and after,
recording.
A.7.1.2 Weigh the sample about 2g, accurate to 0.0001g, tile in the weighing bottle thickness of not more than 5mm, if the sample is crystal, fast
Crushed to 2mm below the small particles, open placed in the oven, the bottle stand next to. At room temperature, reduced to less than 2.67 kPa, and dried
24h After the end of the cover to remove the cap, weighing.
A.7.2 Result calculation
The mass fraction w4 of the drying reduction is calculated according to equation (A.4)
w4 =
m3-m4
m3-m5 ×
100% (A.4)
Where.
m3 --- the quality of the weighing bottle and the sample, in grams (g);
m4 --- the quality of the bottle and the sample after drying, in grams (g);
m5 --- Weigh the quality of the bottle, in grams (g).
The results of the test are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
Value is not greater than 0.2%.
A.8 Determination of burning residue
Weigh the sample about 1g, accurate to 0.0001g. According to the method specified in GB 5009.4.
A.9 Determination of light transmittance
A.9.1 Instruments and equipment
Spectrophotometer.
A.9.2 Analysis steps
Weigh the sample 0.50g, add 10mL water dissolved, shake with 1cm quartz cuvette, water as a blank control, at a wavelength of 430nm
The light transmittance of the sample solution was measured and the reading was recorded.
The results of the test are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
The value is not greater than 0.1%.
A.10 Sulfate (measured in SO4)
A.10.1 Reagents and materials
A.10.1.1 Potassium Sulfate Standard Solution. 0.1 mg/mL.
A.10.1.2 Hydrochloric acid solution. 10%.
A.10.1.3 Barium chloride solution. 1 mol/L.
A.10.2 Analysis steps
Weigh the sample 0.70g, dissolved in water to 40mL (solution, such as alkaline, can be added hydrochloric acid to make neutral; solution if not clear, should be over
Filter), placed in 50mL Na colorimetric tube, add hydrochloric acid solution 2mL, shake, that sample solution. Another take the standard solution of potassium sulfate 2.1mL,
Placed in another 50mL Na colorimetric tube, diluted with water to 40mL, add hydrochloric acid solution 2mL, shake, that is, the standard control solution. in
Sample solution and standard control solution, respectively, by adding barium chloride solution 5mL, diluted with water to 50mL, shake well, placed 10min,
With the same on a black background, from the top of the color tube down to observe, compare.
If the turbidity of the sample solution is not higher than the turbidity of the standard control solution, the sulfate content ≤ 0.03%.
A.11 Ammonium salt (calculated as NH4)
A.11.1 Reagents and materials
A.11.1.1 Magnesium oxide.
A.11.1.2 Ammonium chloride standard solution. 0.01 mg/mL.
A.11.1.3 Ammonia-free distilled water.
A.11.1.4 Hydrochloric acid solution. 10%.
A.11.1.5 Sodium hydroxide solution. Weigh 4.3g of sodium hydroxide, add water and dissolve to 100mL.
A.11.1.6 alkaline potassium iodide solution. take potassium iodide 10g, add water 10mL dissolved, slowly adding mercuric chloride saturated aqueous solution, edge
Add side to stir, to the formation of red precipitate is no longer dissolved, add potassium hydroxide 30g, dissolved, plus mercuric chloride saturated aqueous solution 1mL or
1mL or more, and diluted with the right amount of water to make.200mL, standing, so that precipitation. Take the upper clear solution.
A.11.2 Analysis steps
Weigh the sample 0.10g, set the distillation bottle, add.200mL of ammonia-free distilled water, add magnesium oxide 1g, heating distillation, distillate into the salt
Acid solution 1 drop and ammonia-free distilled water 5mL 50mL Na colorimetric tube, to be distillate up to 40mL, stop the distillation, add sodium hydroxide
Solution 5 drops, plus no ammonia distilled water to 50mL, add alkaline potassium iodide potassium potassium test solution 2mL, shake, placed 15min that sample solution. Take another
Ammonium chloride standard solution 2 mL A standard control solution was prepared as described above.
If the color of the sample solution is not deeper than the color of the standard tube solution, the ammonium salt content is less than or equal to 0.02%.
A.12 Determination of other amino acids
A.12.1 Reagents and materials
A.12.1.1 N-ethylmaleimidimide ethanol solution. weighed 4.0 g of N-ethylmaleimide, as the 100 mL volumetric flask,
Add 10mL of ethanol dissolved, diluted to the mark.
A.12.1.2 Acetic acid solution. 2 mol/L.
A.12.1.3 n-butanol-acetic acid solution of ninhydrin. 0.2 g of ninhydrin was weighed into a 100 mL volumetric flask and 5.0 mL of acetic acid was added and
Plus n-butanol dissolved and diluted to the mark.
A.12.1.4 L-cysteine hydrochloride monohydrate standard.
A.12.1.5 Tyrosine standards.
A.12.1.6 Expanding agent. glacial acetic acid. water. n-butanol = 1. 1. 3.
A.12.1.7 L-cysteine hydrochloride standard stock solution. take L-cysteine hydrochloride - water standard 20mg, add water 10mL dissolved
Solution, plus N-ethyl maleimide imide ethanol solution 10mL, mix, place 5min.
A.12.1.8 System Applicability Test Solution. Take tyrosine standard 10mg, placed in 25mL volumetric flask, add water to dissolve, add L-half
Cystine hydrochloride standard stock solution 10mL, diluted with water to the mark, shake.
A.12.2 Analysis steps
Weigh the sample 0.20g, placed in 10mL volumetric flask, add water and dilute to the mark, shake, the amount of 5mL, plus N-ethyl
5ml allylene ethanol solution, mix and place for 5 min. That sample solution. Accurately measure the sample solution 1mL, placed in.200mL
Capacity bottle, diluted with water to the mark, shake. That is, the control solution.
Take the sample solution, the control solution and the system suitability test solution each 5μL, respectively, points on the same silica gel G plate to expand agent
Expand at least 15cm, start, dry, heat at 80 ℃ for 30min, spray ninhydrin-acetic acid solution of ninhydrin, heating at about 105 ℃
15min to spot appear, view immediately.
System suitability test solution should be two completely separate spots, the control solution should be a clear spot, otherwise the test results
effect. Sample solutions such as display spots, stains and the control solution of the spots compared to the spot should not be deeper.
A.13 Determination of iron salts (in terms of Fe)
A.13.1 Reagents and materials
A.13.1.1 Ammonium persulfate.
A.13.1.2 n-butanol.
A.13.1.3 iron standard solution. weighed ammonium ferric sulfate [FeNH4 (SO4) 2 · 12H2O] 0.863g, placed in a 1000mL volumetric flask, add water
After dissolving, add 2.5mL of sulfuric acid, diluted with water to the mark, shake, as the stock solution. Before use, the precise amount of liquid storage system 10mL, placed
100mL volumetric flask, diluted with water to the mark, shake (1mL each equivalent to 10μg of Fe2).
A.13.1.4 iron standard solution. precise amount of iron standard stock solution 10mL, placed in 100mL volumetric flask, diluted with water to the mark, shake.
A.13.1.5 Hydrochloric acid solution. 10%.
A.13.1.6 Ammonium thiocyanate solution. 30%.
A.13.2 Analysis steps
Weigh the sample 1.0g, dissolved in water to 25mL, displaced 50mL Na colorimetric tube, hydrochloric acid solution 4mL and ammonium persulfate
0.05g, diluted with water into 35mL, add ammonium thiocyanate solution 3mL, add water diluted to 50mL, shake, that is, the sample solution.
Another 1.0mL iron standard solution, placed in another 50mL Nessler colorimetric tube, add water to 25mL, add hydrochloric acid solution 4mL and sulfur
Ammonium nitrate 0.05g, diluted with water to 35mL, add ammonium thiocyanate solution 3mL, add water diluted to 50mL, shake, that was control
Solution.
Sample solution such as color, immediately compared with the control solution, the color should not be deeper. If the sample solution is inconsistent with the color of the control solution,
Were transferred to the separatory funnel, the addition of n-butanol 20mL extraction, to be layered, the n-butanol layer was placed 50mL Nessler colorimetric tube, and then
N-butanol diluted to 25mL, the sample solution compared with the control solution, the color should not be deeper.
A.14 Determination of heavy metals (Pb)
A.14.1 Reagents and materials
A.14.1.1 nitric acid.
A.14.1.2 lead standard stock solution. take 0.160g lead nitrate, 1000mL volumetric flask, add nitric acid 5mL and water 50mL dissolved,
Diluted with water to the mark, shake, configuration and storage of glass containers are not lead.
A.14.1.3 lead standard solution. the precise amount of standard lead reserves of 10mL, set 100mL volumetric flask, diluted with water to the mark, shake, with
The glass containers for storage and storage shall not contain lead.
A.14.1.4 acetic acid solution. take acetic acid 60mL, diluted with water to 1000mL.
A.14.1.5 sodium sulfide solution. take sodium sulfide 1g, add water to dissolve into 10mL, the liquid should be temporary with the new system.
A.14.1.6 Ammonia solution. take concentrated ammonia solution 400mL, diluted with water to 1000mL.
A.14.2 Instruments and equipment
A.14.2.1 Nessler Colorimetric tubes. 100 mL.
A.14.2.2 Filter paper. Φ = 1.2 μm.
A.14.3 Analysis steps
Weigh 2.0 g of the sample, placed in the Nessler color tube, dissolved in 10mL water and adjusted to 7.0 with ammonia solution, plus 2mL of acetic acid
Solution, add water to 40mL, shake, if the solution is not clear, filter with filter paper, add water to 50mL. Take 2.0mL lead standard solution at the same time
For each tube in a drop of sodium sulfide test solution, shake, store 5min, in contrast to the color on a white background. The color of the sample solution is mixed with the standard solution
Liquid color contrast should not be deeper.
A.15 Determination of arsenic (As)
A.15.1 Reagents and materials
A.15.1.1 Zinc pellets. The zinc particles used in this method should be arsenic free to be able to pass fine particles of the No. 1 sieve.
A.15.1.2 lead acetate cotton. take absorbent cotton 1.0g, immersed in lead acetate test solution and water isovolumetric mixture of 12mL, wet, squeeze in addition to
To the excess solution, and make it loose, dry at 100 ℃ below, stored in a glass stopper in reserve.
A.15.1.3 Mercury bromide test paper. take the filter paper immersed in ethanol bromide solution (50g/L), 1h after removal, dry in the dark.
A.15.1.4 Concentrated hydrochloric acid.
A.15.1.5 dilute sulfuric acid. the amount of sulfuric acid to take 57mL, diluted with water to 1000mL.
A.15.1.6 arsenic standard stock solution. take arsenic trioxide 0.132g, set 1000mL volumetric flask, add 20% sodium hydroxide solution 5mL dissolved
Solution, with the amount of dilute sulfuric acid and then add dilute sulfuric acid 10mL, diluted with water to the mark, shake.
A.15.1.7 arsenic standard solution. the precise amount of arsenic standard stock solution 10mL, set 1000mL volumetric flask, add dilute sulfuric acid 10mL, dilute with water
Release to the scale, shake.
A.15.1.8 acidic stannous chloride solution. take stannous chloride 20g, concentrated hydrochloric acid to dissolve and volume to 50mL, filtration. Shelf life
3 months.
A.15.1.9 potassium iodide solution. take potassium iodide 16.5g, add water to dissolve and set to 100mL.
A.15.1.10 Lead acetate solution. take lead acetate 10g, add a new boiling cold water dissolved, add acetic acid to clarify the solution, plus the new boiling
Cold water to make 100mL.
A.15.2 Instruments and equipment
A.15.2.1 No. 1 sieve. sieve diameter (average).2000μm ± 70μm (10 mesh).
A.15.2.2 Reaction bottle. As shown in Figure A.1, A is a 100 mL standard grinding conical flask; B is a hollow standard grinding plug,
C (outer diameter 8.0mm, inner diameter 6.0mm), full length of about 180mm; D for the porous plexiglass cocks, the upper part of the circular plane, the central
A hole having an aperture corresponding to the inner diameter of the air guide pipe C and a lower aperture corresponding to the outer diameter of the air guide pipe C,
And the tube wall is aligned with the round hole of the cock, and the adhesive is fixed. E is the organ glass whisker with a circular hole (pore size 6.0mm)
Plug cover, and D close match.
The unit is in millimeters
Figure A.1 Reaction bottle equipment
Test, in the air pipe C into the lead acetate cotton 60mg (tube height of 60mm ~ 80mm), and then the top of the cock D
Place a piece of mercury bromide on paper (the size of the test paper to cover the aperture without falling out of the plane is appropriate), cover the plug cover E and tighten.
A.15.3 Analysis steps
Weigh 2.0g of the sample, placed in the reaction flask, add hydrochloric acid 5mL and water 21mL, then add potassium iodide test solution 5mL, and then add acid
5 drops of stannous chloride solution, placed at room temperature for 10min, add zinc particles 2g, immediately the gas pipe on the reaction bottle, and the reaction bottle set
25 ℃ ~ 40 ℃ water bath, the reaction 45min, remove the mercury bromide test paper. Another 2mL of arsenic standard solution at the same time operation, colorimetric. Sample dissolved
The color of the arsenic produced by the liquid is compared with the color of the arsenic produced by the standard solution and should not be deeper.
Arsenic standard solution generated arsenic must be significant color, otherwise the test results are invalid.
Appendix B
L-cysteine hydrochloride monohydrate standard infrared spectroscopy
The standard infrared spectra of L-cysteine hydrochloride monohydrate are shown in Figure B.1.
Figure B.1 L-cysteine hydrochloride monohydrate standard infrared spectroscopy (potassium bromide compression method)
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