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GB 28309-2012: Food Additives Acid Red (azo Indirubin)
Status: Valid
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GB 28309-2012439 Add to Cart 4 days Food Additives Acid Red (azo Indirubin) Valid

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Basic data

Standard ID: GB 28309-2012 (GB28309-2012)
Description (Translated English): Food Additives Acid Red (azo Indirubin)
Sector / Industry: National Standard
Classification of Chinese Standard: C54;X40
Classification of International Standard: 67.220.20
Word Count Estimation: 19,133
Regulation (derived from): Ministry of Health Bulletin No. 7 of 2012
Issuing agency(ies): Ministry of Health of the People's Republic of China
Summary: This Chinese standard applies to 1-naphthylamine-4 sulfonate by diazotization with a 1-naphthylamine-4 Sodium coupling obtained food additives Acid Red (Azo Rubine).

GB 28309-2012: Food Additives Acid Red (azo Indirubin)

---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 Additives Acid Red (azo Indirubin) National Standards of People's Republic of China National standards for food safety Food Additives Acid Red (Azo-Red) 2012-04-25 release 2012-06-25 Implementation Issued by the Ministry of Health of the People's Republic of China National standards for food safety Food Additives Acid Red (Azo-Red)

1 Scope

This standard applies to 1-naphthylamine-4-sulfonic acid sodium diazotization and 1-naphthol-4-sulfonate coupling and the preparation of food additives acid red (even Nitrogen jade red). 2 Chemical name, structural formula, molecular formula and relative molecular mass 2.1 Chemical name 1-hydroxy-2- (4-azo naphthalenesulfonic acid) -4-naphthalenesulfonic acid disodium salt 2.2 Structural formula 2.3 Molecular formula C20H12N2Na2O7S2 2.4 Relative molecular mass 502.43 (according to the.2007 International Relative Atomic Quality)

3 technical requirements

3.1 sensory requirements. should be consistent with the provisions of Table 1. Table 1 sensory requirements The project requires a test method Color reddish brown to dark reddish brown State powder or particles Take the appropriate amount of sample placed in a clean, dry white porcelain dish, in the natural light, Observe its color and state 3.2 Physical and chemical indicators. should be consistent with the provisions of Table 2. Table 2 Physical and chemical indicators Item Index Test Method Acid red (azo-erythropo red) content, w /% ≥ 85.0 Appendix A, A.3 Dry reduction, chloride (in terms of NaCl) and sulfate ≤ (In terms of Na2SO4), w /% 15.0 Appendix A, A.4 Water insoluble matter, w /% ≤ 0.20 Appendix A, A.5 Sub-dye, w /% ≤ 1.0 Appendix A A.6 The sum of the unreacted raw materials, w /% ≤ 0.50 A.7 in Appendix A Unsulfonated aromatic primary amine (in aniline), w /% ≤ 0.01 A.8 in Appendix A. Total arsenic (in As)/(mg/kg) ≤ 1.0 GB/T 5009.11 Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.12

Appendix A

Testing method A.1 General provisions The reagents and water used in this standard, when not specified in other requirements, refers to the analysis of pure reagents and GB/T 6682-2008 of the three water. Standard solution used in the test, the standard solution of impurities, preparations and products, in the absence of other requirements, according to GB/T 601, GB/T 602, GB/T 603. The solution used in the experiment, when not specified with the preparation of the solvent, refers to the aqueous solution. A.2 Identification test A.2.1 Reagents and materials A.2.1.1 Sulfuric acid. A.2.1.2 Ammonium acetate solution. 1.5 g/L. A.2.2 Instruments and equipment A.2.2.1 Spectrophotometer. A.2.2.2 Cuvette. 10mm. A.2.3 Identification method A.2.3.1 Weigh about 0.1g of sample, accurate to 0.01g, dissolved in 100mL water, the solution is clear red. A.2.3.2 Weigh about 0.1g sample, accurate to 0.01g, add 10mL sulfuric acid, the solution was red, take this solution 2 to 3 drops in 5mL water , The solution was red. A.2.3.3 Weigh about 0.1g sample, accurate to 0.01g, dissolved in 100mL ammonium acetate solution, take 1mL of this solution, add ammonium acetate solution Liquid to 100 mL, and the maximum absorption wavelength of the solution is 516 nm ± 2 nm. A.3 Determination of acid red (azo-erythropoene) content A.3.1 Titanium trichloride titration (Arbitration) A.3.1.1 Method Summary In the acidic medium, the azo group in the acid red (azo-erythropo red) is reduced and decomposed by titanium trichloride, and the solution is titrated according to the standard titration solution of titanium trichloride Consumption, calculate the acid red (azo jade red) content. A.3.1.2 Reagents and materials A.3.1.2.1 trisodium citrate. A.3.1.2.2 Titanium trichloride standard titration solution. c (TiCl3) = 0.1mol/L (now with the use of the preparation method see Appendix B). A.3.1.2.3 Carbon dioxide. A.3.1.3 Instruments and equipment See Figure A.1. A - conical flask (500mL); B - brown burette (50mL); C --- black paper with black paper bottle (2000mL); D - container (5000 mL) containing 100 g/L ammonium carbonate solution and 100 g/L ferrous sulfate solution in equal volume; E --- piston F - empty bottle; G --- water washing gas bottle. Figure A.1 Titanium trichloride titration device A.3.1.4 Analysis steps Approximately 0.5 g of the sample was weighed to 0.0001 g, placed in a 500 mL Erlenmeyer flask, 50 mL of freshly boiled and cooled to room temperature Water, dissolve, add 15g trisodium citrate and 150mL fresh boil and cool to room temperature water, shake dissolved, according to Figure A.1 installed the instrument, While the carbon dioxide is fed under the liquid level, it is heated to boiling and titrated with titanium titanate titration solution until its inherent color disappears as the end point. A.3.1.5 Calculation of results Acid red (azo-erythropo red) content in mass fraction w1, the value in%, calculated according to formula (A.1). w1 = c (V/1000) (M/4) m1 × 100% (A.1) Where. c - Titanium trichloride standard titration solution concentration of the exact value in moles per liter (mol/L); V --- titration sample consumption of titanium trichloride standard titration solution volume of the exact value in milliliters (mL); 1000 --- volume conversion factor; M is the molar mass of acid red (azo-erythropo red) in grams per mole (g/mol) [M (C20H12N2Na2O7S2) = 502.43]; 4 --- concentration conversion factor; m1 --- the value of the sample quality, in grams (g). The experimental results are based on the arithmetic mean of the parallel measurement results (leave a decimal). Two independent tests obtained under repetitive conditions The absolute difference between the results is not more than 1.0%. A.3.2 Spectrophotometric colorimetric method A.3.2.1 Methodological Summary The sample and the known content of acid red (azo-yu red) standard were dissolved in water, diluted with ammonium acetate solution volume, the maximum suction Close the wavelength, respectively, measured its absorbance value, and then calculate its content. A.3.2.2 Reagents and materials A.3.2.2.1 Ammonium acetate solution. 1.5 g/L. A.3.2.2.2 Acid red (azo jade red) Standard. ≥85.0% (mass fraction, measured according to A.3.1). A.3.2.3 Instruments and equipment A.3.2.3.1 Spectrophotometer. A.3.2.3.2 Cuvette. 10mm. A.3.2.4 Analysis steps A.3.2.4.1 Preparation of Acid Red (Azo-Red) Standard Solution Weigh about 0.25g acid red (azo jade red) standard, accurate to 0.0001g, dissolved in water, into the 1000mL volumetric flask In the water diluted and fixed to the scale, shake. Absorb 10mL, into the 500mL volumetric flask, add ammonium acetate solution diluted and constant volume to the moment Degree, shake, spare. A.3.2.4.2 Preparation of Acid Red (Azo-Red) Sample Solution Weighing and operating methods with A.3.2.4.1 standard solution preparation. A.3.2.4.3 Determination Take the appropriate amount of acid red (azo jade red) standard solution and acid red (azo jade red) sample solution, were placed in 10mm cuvette, the same The respective absorbance values were measured with a spectrophotometer at the maximum absorption wavelength (516 nm ± 2 nm), and the ammonium acetate solution was used as the reference solution. A.3.2.5 Calculation of results Acid red (azo-erythropo red) content in mass fraction w2, the value in%, according to formula (A.2) calculation. w2 = Am0A0m × w0 (A.2) Where. A - acid red (azo jade red) sample solution absorbance value; m0 --- acid red (azo-red) standard product quality value, the unit is grams (g); A0 --- acid red (azo jade red) standard solution absorbance value; m - the mass of the sample, in grams (g); w0 --- acid red (azo jade red) standard content of the value,%. The experimental results are based on the arithmetic mean of the parallel measurement results (leave a decimal). Two independent tests obtained under repetitive conditions The absolute difference between the results is not more than 1.0%. A.4 Determination of dry reduction, total amount of chloride (in terms of NaCl) and sulfate (calculated as Na2SO4) A.4.1 Determination of dry reduction A.4.1.1 Analysis steps Weigh about 2g sample, accurate to 0.001g, placed in 135 ℃ ± 2 ℃ constant temperature drying box constant weighing bottle, at 135 ℃ ± 2 ℃ Constant temperature drying oven to constant volume. A.4.1.2 Calculation of results The drying loss is expressed in terms of mass fraction w3 and the value in%, calculated according to formula (A.3) w3 = m2-m3m2 × 100% (A.3) Where. m2 --- the value of the sample before drying, in grams (g); m3 --- the value of the sample after drying to constant volume, in grams (g). The experimental results are based on the arithmetic mean of the parallel measurement results (leave a decimal). Two independent tests obtained under repetitive conditions The absolute difference between the results is not more than 0.2%. A.4.2 Determination of chloride (in terms of NaCl) A.4.2.1 Reagents and materials A.4.2.1.1 Nitrobenzene. A.4.2.1.2 Activated carbon. 767 needle type. A.4.2.1.3 Nitric acid solution. 1 1. A.4.2.1.4 Silver nitrate solution. c (AgNO3) = 0.1 mol/L. A.4.2.1.5 ammonium ferric sulfate solution. Weigh about 14g ammonium ferric sulfate, dissolved in 100mL water, filtered, add 10mL nitric acid, stored in brown Color bottle. A.4.2.1.6 Ammonium thiocyanate standard titration solution. c (NH4CNS) = 0.1mol/L. A.4.2.2 Analysis steps A.4.2.2.1 Preparation of sample solution Weigh about 2g sample, accurate to 0.001g, dissolved in 150mL water, add about 15g activated carbon, gently boil 2min ~ 3min, plus Into 1mL nitric acid solution, constantly shaking evenly, placed 30min (during which time shaking). Filter with dry filter paper. If the filtrate is colored, then again Add 5g activated carbon, from time to time shaking under 1h, and then filter the dry filter paper (if there is still color is replaced by activated carbon repeated operation to the filtrate colorless). Each time to 10mL water activated carbon three times, the filtrate combined into the.200mL volumetric flask, add water to the mark, shake. For chlorides and sulfur Determination of acid salt content. A.4.2.2.2 Determination Remove the 50 mL sample solution, place in a 500 mL Erlenmeyer flask, add 2 mL of nitric acid solution and 10 mL of silver nitrate solution (chloride containing The amount of time to add more) and 5mL nitrobenzene, shake to silver chloride condensation, add 1mL ammonium ferric sulfate solution, with ammonium thiocyanate standard Titration solution titrated excess silver nitrate to the end and hold for 1 min, while the same method to do a blank test. A.4.2.3 Calculation of results Chloride (in terms of NaCl) is expressed as a mass fraction of w4, expressed in%, calculated according to formula (A.4) w4 = c1 [(V1-V0)/1000] M1 m4 (50/200) x 100% (A.4) Where. c1 --- ammonium thiocyanate standard titration solution concentration of the exact value, the unit is mol per liter (mol/L); V1 --- titration blank solution consumption of ammonium thiocyanate standard titration solution volume of the exact value in milliliters (mL); V0 --- titration sample solution consumption of ammonium thiocyanate standard titration solution volume of the exact value in milliliters (mL); 1000 --- volume conversion factor; M1 --- sodium chloride molar mass value in grams per mole (g/mol) [M1 (NaCl) = 58.4]; m4 --- the value of the sample quality, in grams (g); 50/200 --- dilution factor. The experimental results are based on the arithmetic mean of the parallel measurement results (leave a decimal). Two independent tests obtained under repetitive conditions The absolute difference between the results is not more than 0.3%. A.4.3 Determination of Sulfate (calculated as Na2SO4) A.4.3.1 Reagents and materials A.4.3.1.1 Sodium hydroxide solution. 0.2 g/L. A.4.3.1.2 Hydrochloric acid solution. 1 99. A.4.3.1.3 barium chloride standard titration solution. c (1/2BaCl2) = 0.1mol/L (see Appendix C for the preparation method). A.4.3.1.4 phenolphthalein indicator solution. 10g/L. A.4.3.1.5 Sodium Roseate Indicator. Weigh 0.1 g of sodium rosin sodium and dissolve in 10 mL of water (now available). A.4.3.2 Analysis steps Absorb 25mL sample solution (A.4.2.2.1), placed in 250mL Erlenmeyer flask, add 1 drop of phenolphthalein indicator solution, add sodium hydroxide solution Liquid was pink, and then dropping hydrochloric acid solution to pink disappeared, shake, dissolved in the constant shaking with barium chloride standard titration solution titration, With sodium alanate indicator liquid for the external indicator solution, the reaction solution and indicator liquid on the filter paper at the intersection of rose red spots and keep 2min Fade for the end. While the same method to do blank test. A.4.3.3 Calculation of results The content of sulfate (in terms of Na2SO4) is expressed in terms of mass fraction w5 and the value in%, calculated according to formula (A.5) w5 = c2 [(V2-V3)/1000] (M2/2) m5 (25/200) x 100% (A.5) Where. c2 --- barium chloride standard titration solution concentration of the exact value in moles per liter (mol/L); V2 --- titration sample solution consumption of barium chloride standard titration solution volume of the exact value in milliliters (mL); V3 --- titration blank solution consumption of barium chloride standard titration solution volume of the exact value in milliliters (mL); 1000 --- volume conversion factor; (G/mol) [M2 (Na2SO4) = 142.04]; the mass of the mass fraction of sodium sulfate, 2 --- concentration conversion factor; m5 --- the mass of the sample, in grams (g); 25/200 --- dilution factor. The experimental results are based on the arithmetic mean of the parallel measurement results (leave a decimal). Two independent tests obtained under repetitive conditions The absolute difference between the results is not more than 0.2%. A.4.4 Calculation of dry reduction, chloride (calculated as NaCl) and sulfate (calculated as Na2SO4) The total amount of dry reduction, chloride (in terms of NaCl) and sulfate (calculated as Na2SO4) is expressed in terms of mass fraction w6, expressed as% Calculated according to formula (A.6). w6 = w3 w4 w5 (A.6) Where. w3 --- dry reduction,%; w4 --- chloride (in terms of NaCl) content,%; w5 --- sulfate (in Na2SO4 dollars) content,%. A.5 Determination of water insoluble matter A.5.1 Instruments and equipment A.5.1.1 Glass sand core crucible. G4, pore size of 5μm ~ 15μm. A.5.1.2 Constant temperature oven. A.5.2 Analysis steps Weigh about 3g sample, accurate to 0.001g, placed in 500mL beaker, add 50 ℃ ~ 60 ℃ hot water 250mL, so that dissolved, The mixture was filtered through a G4 glass sand core crucible which had been baked at 135 ° C ± 2 ° C and kept constant and washed with hot water until the washing solution was colorless at 135 ° C ± 2 ° C Constant temperature drying oven to constant volume. A.5.3 Calculation of results Water insoluble matter in mass fraction w7, the value in%, according to formula (A.7). w7 = m6m7 × 100% (A.7) Where. m6 --- the value of the water insoluble matter after drying, in grams (g); m7 --- the value of the sample quality, in grams (g). The experimental results are based on the arithmetic mean of the parallel measurement results (whichever is two decimal places). Two independent tests obtained under repetitive conditions The absolute difference between the results is not more than 0.05%. A.6 Determination of secondary dyes A.6.1 Methodological summary The components were separated, eluted and then quantitated by spectrophotometry. A.6.2 Reagents and materials A.6.2.1 anhydrous ethanol. A.6.2.2 n-butanol. A.6.2.3 Acetone solution. 1 1. A.6.2.4 Ammonia solution. 4 96. A.6.2.5 Sodium bicarbonate solution. 4 g/L. A.6.3 Instruments and equipment A.6.3.1 Spectrophotometer. A.6.3.2 chromatography filter paper. No. 1 medium speed, 150mm × 250mm. A.6.3.3 chromatography cylinder. φ240mm × 300mm. A.6.3.4 Micro Sampler. 100 μL. A.6.3.5 Nessler's colorimetric tube. 50mL with a glass grinder. A.6.3.6 glass sand core funnel. G3, aperture of 15μm ~ 40μm. A.6.3.7 50mm cuvette. A.6.3.8 10mm cuvette. A.6.4 Analysis steps A.6.4.1 Paper chromatography conditions A.6.4.1.1 Expanding agent. n-butanol anhydrous ethanol ammonia solution = 6 2 3. A.6.4.1.2 Temperature. 20 ° C to 25 ° C. A.6.4.2 Preparation of sample solution Weigh 1g sample, accurate to 0.001g, placed in a beaker, add the appropriate amount of water dissolved, into the 100mL volumetric flask, diluted to the moment The amount of the sample solution is 1%. A.6.4.3 Preparation of sample eluate Use a micro-injector to draw 100 μL of the sample solution, evenly on a bottom line of 25 mm from the bottom of the filter paper, Its width in the filter paper does not exceed 5mm, length of 130mm, with a hair dryer to dry. Place the filter paper in a pre-formulated developer Of the column, the bottom edge of the filter paper immersed in the developer under the liquid surface 10mm, until the agent before the line rose to 150mm or until the dye Separated from satisfaction. Remove the filter paper, dry with cold air. With the blank filter paper under the same conditions to expand, the blank filter paper must be carried out with the above steps to use the filter paper on the same filter paper on the adjacent Bit cut. The chromatogram of the secondary dye paper is shown in Figure A.2. Figure A.2 Schematic diagram of chromatographic analysis of secondary dyes The respective sub-dyes obtained after the development and the filter paper on the blank filter paper corresponding to the respective sub-dyes are cut in the same size and Cut into about 5mm × 15mm thin strips, were placed in 50mL Na colorimetric tube, accurately add 5mL acetone solution, shake 3min ~ 5min, and then accurately add 20mL sodium bicarbonate solution, shake, and then in the G3 glass sand core funnel naturally Filter, the filtrate must be clear, no suspended solids. Respectively, to obtain the secondary dye and blank eluent. At the maximum absorption wavelength of the respective sub-dyes, The eluent of each sub-dye was measured on a spectrophotometer using a 50 mm cuvette. When the absorbance was measured on a spectrophotometer, a mixture of 5 mL of acetone solution and 20 mL of sodium bicarbonate solution was used as the reference solution. A.6.4.4 Preparation of standard solutions Absorb 2mL 1% of the sample solution into the 100mL volumetric flask, diluted to the mark, shake, the solution as the standard solution. A.6.4.5 Preparation of standard eluate Use a micro-injector to draw 100 μL of the standard solution, evenly point on the bottom of the filter paper 25mm on a baseline, with a hair dryer blowing dry. The filter paper into a pre-prepared with a good preparation agent in the chromatography cylinder to start, before the agent to rise 40mm, take out with cold air blowing Dry, cut all the expanded part of the dye, according to the method of A.6.4.3 extraction operation, get the standard eluent. With 10mm cuvette Measure the absorbance at the maximum absorption wavelength. At the same time with the blank filter paper under the same conditions to expand, according to the same method after the test wash the absorbance value. A.6.4.6 Calculation of results The content of the secondary dye is expressed in terms of mass fraction w8 and the value in%, calculated according to the formula (A.8) w8 = [(A1-b1) (An-bn)]/5 (AS-bS)......
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