Some standard content:
GB 17511.1—1998
This standard is equivalent to the "Japanese Food Additives Standard (1992 Sixth Edition)", and is formulated based on the "Food Red No. 40 (Allure Red) Standard" in the book.
The main differences between this standard and the Japanese standard are as follows: 1. In addition to the titanium trifluoride titration method, the spectrophotometry method is added to the product content determination in this standard. This method is used as the daily determination method, and the titanium trichloride method is used as the arbitration method.
2. The total amount of loss on drying, chloride (calculated as NaCl) and sulfate (calculated as NazSO) in this standard is <15.0%, and this standard is divided into the loss on drying index of ≤10.0%, and the chloride and sulfate indexes of ≤5.0%. 3. The determination method of chloride (calculated as NaCl) and sulfate (calculated as NaSO.) in this standard is chemical titration, while the Japanese standard adopts ion chromatography.||tt ||4. The content of arsenic in this standard is determined according to GB/T8450-1987 "Determination of Arsenic in Food Additives", with an index of ≤0.0001% (As) and a Japanese index of ≤0.0004% (As20.). Appendix A of this standard is the appendix of the standard.
This standard was proposed by the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the dye standardization technical unit of the former Ministry of Chemical Industry and the Food Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by the Shanghai Dye Research Institute and the Health Supervision Institute of the Shanghai Municipal Health Bureau. The main drafters of this standard are: Ding Deyi, Sheng Bangguo, Di Jinjun, Ying Huiru, Shi Huaijiong, Zhou Yanqin. This standard is entrusted to the dye standardization technical unit of the former Ministry of Chemical Industry for interpretation. 519
1 Scope
National Standard of the People's Republic of China
Food Additives
Allura Red
Food additive
Fancy(Allura) red
GB 17511. 1— 1998
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation and storage of food additives for allergic red. This standard applies to dyes formed by coupling 4-amino-5-methoxy-2-methylbenzenesulfonic acid with sodium 6-hydroxy-2-naphthalenesulfonate after diazotization. This product can be added to food as a colorant. Structural formula:
Molecular formula: C:HN,Na2O.S2
Relative molecular mass: 496.43 (according to the 1995 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. 8 Preparation of difficult solutions for titration analysis (volume analysis) of chemical reagents GB/T 601--1988
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 602—19881
GB/T 603—1988
Preparation of preparations and products used in chemical reagent test methods Specifications and test methods for water for analytical laboratories (neqISO3696:1987) GB/T 6682-—1992
GB/T 8450--1987
3 Requirements
Determination of arsenic in food additives
3.1 Appearance: This product is dark red powder.
3.2 Food additives Sensitive red should meet the requirements of Table 1: Approved by the State Administration of Quality and Technical Supervision on October 19, 1998 520
Implemented on April 1, 1999
Loss on drying, total amount of chloride (calculated as NaCl) and sulfate (calculated as Na2SO,)
Water insoluble matter
Low sulfonated secondary dye
High sulfonated secondary dye
GB 17511. 11998
Table 1 Requirements
6-Hydroxy-5-[2-methoxy-5-methyl-4-sulfonylbenzene)azo]-8-(2-methoxy-5-methyl-4-sulfonylphenoxy)-2-naphthalenesulfonic acid disodium salt 6-hydroxy-2-naphthalenesulfonic acid sodium salt
4-Amino-5-methoxy-2-methylbenzenesulfonic acid 6.5\-oxo-bis(2-bansulfonic acid) disodium salt Unsulfonated aromatic primary amines (calculated as aniline)
Arsenic (As)
Heavy metals (calculated as Pb)
Lead (Pb)
4 Test methods
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB/T 6682. The standard solutions, impurity standard solutions, preparations and products required in the test shall be prepared in accordance with the provisions of GB/T601.GB, T602 and GB/T603 unless otherwise specified.
4.1 Appearance
Visual inspection.
4.2 Identification
4.2.7 Reagents and materials
a) Sulfuric acid solution: 1+100;
b) Ammonium acetate solution: 1.5g/L.
4.2.2 Instruments and equipment
Spectrophotometer.
4.2.3 Test method
4.2.3.1 Weigh about 0.1g of the sample and dissolve it in 1000mL of water to form a red clear solution. 4.2.3.2 Take 40 mL of the red clear solution in 4.2.3.1, add 10 mL of sulfuric acid solution, the solution turns dark purple, take 2-3 drops of this solution and add it to 5 mL of water, it turns red.
4.2.3.3 Weigh 0.1 g of the sample, dissolve it in 100 mL of ammonium acetate solution, take 1 mL of this solution and add ammonium acetate solution to 100 mL, the maximum absorption wavelength of the solution is 499 nm ± 2 nm. 4.3 Determination of allura red content
4.3.1 Titanium trifluoride titration method (arbitration method) 4.3.1.1 Summary of the method
In an alkaline medium, the azo group in the dye is reduced and decomposed into an amino compound by titanium trichloride, and the percentage of the dye is calculated according to the consumption of titanium trichloride standard titration solution.
4.3.1.2 Reagents and materials
a) Trisodium citrate;
GB 17511. 1 -- 1998
b) Standard solution of titanium trichloride: c(TiCl)=0.1mol/L, freshly prepared. See Appendix A (Appendix of the standard) for the preparation method; c) Carbon dioxide in a cylinder.
4.3.1.3 Analysis steps
Weigh about 5g of the sample, accurate to 0.0002g. Dissolve in 100mL of freshly boiled and cooled distilled water, transfer to a 500mL volumetric flask, dilute to the mark, and shake to hook. Pipet 50mL, place in a 500mL conical flask, add 15g of trisodium citrate and 150mL of water. Assemble the instrument according to Figure 1, heat to boiling while passing a stream of carbon dioxide gas below the liquid surface, and titrate with titanium trifluoride standard solution until the colorless end point.
4.3.1.4 Expression of analysis results
Mass percentage of allura red X: calculated according to formula (1): Vc×0.124 1 × 100
m×500
Wherein: V—volume of titanium trichloride standard solution consumed in titration of sample, mL; actual concentration of titanium trichloride standard solution, mol/L; 0. 124 1-
（1）
Mass of allura red equivalent to 1.00ml titanium trifluoride standard titration solution [c(TiCl)=1.000mol/L] in grams:
Mass of sample, starting.
4.3.1.5 Allowable difference
The difference between two parallel determination results shall not exceed 1%, and their arithmetic mean shall be taken as the determination result. 4.3.2 Spectrophotometric colorimetric method
4.3.2.1 Method summary
After making solutions of the sample and the standard sample with known content, measure their absorbance at the maximum absorption wavelength, and then calculate the content of the sample.
1-1 conical flask (500mL);2-brown burette (50mL)3-bottom glass bottle wrapped with black paper (2000mL);4-conical container containing 100g/L ferrous carbonate and 100g/L ferrous sulfate in equal amounts (5000mL);5-piston:6-empty bottle:7-washing bottle filled with waterFigure 1 Apparatus diagram of titanium trichloride titration method
4.3.2.2 Reagents and materials
Ammonium acetate solution: 1.5g/L.
4.3.2.3 Instruments and equipment
a) Spectrophotometer;
b) Cuvette: 10 mm.
4.3.2.4 Preparation of Allura Red Standard Solution
GB 17511. 1—1998
Weigh 0.5 g of Allura Red standard sample, accurate to 0.0002g, dissolved in 1000mL ammonium acetate solution. Take 10ml of this solution, add ammonium acetate solution to 500mL
4.3.2.5 Preparation of allura red test solution
Same as the preparation of standard solution.
4.3.2.6 Test method
Put the standard solution and test solution in 10mm colorimetric blood, and measure the absorbance of each at a wavelength of 499nm±2nm using a spectrophotometer.
Use ammonium acetate solution as the reference solution.
4.3.2.7 Expression of analysis results
The mass percentage of allura red, X, is calculated according to formula (2): X.
Where: A—absorbance of test solution;
A.—absorbance of standard solution;
X,——mass percentage of allura red standard sample (titanium trichloride method). 4.3.2.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of loss on drying, total amount of chloride (calculated as NaCl) and sulfate (calculated as Na2SO4.4.1 Determination of loss on drying
++++(2)
4.4.1.1 Analysis steps
Weigh about 2g of sample to an accuracy of 0.01g, place it in a weighing bottle with a diameter of $(30~40)mm that has been constant weight, and dry it in a constant temperature oven at 135℃±2C to constant weight.
4.4.1.2 Expression of analysis results
Mass percentage of loss on drying X. Calculate according to formula 3): X; = m = m × 100
Wherein: m—-mass of the sample before drying, g;; mass of the sample after drying to constant weight, g
4.4.1.3 Allowable difference
The difference between the results of two parallel measurements shall not exceed 0.2%. The arithmetic mean shall be taken as the measurement result. 4.4.2 Determination of fluoride (as NaCl) content 4.4.2.1 Reagents and materials
a) Activated carbon:
b) Nitrobenzene;
c) Nitric acid solution: 1-1;
d) Silver nitrate standard solution: cAgNO,) = 0.1 mol/I.; e) Ammonium thiosulfate standard solution: c(NH,CNS) = 0.1 mol/LF (3)
f) Ammonium ferric sulfate solution:
GB 17511. 1—1998
Preparation: Weigh 14 g of ammonium ferric sulfate, dissolve it in 100 mL of water, filter, add 10 mL of nitric acid, and store in a brown bottle. 4.4.2.2 Preparation of test solution
Weigh about 2g of the sample, accurate to 0.001g, and accurately add 200mL of water. Add 10g of activated carbon, and then add 1mL of nitric acid, stir evenly, and place for 30min (stir constantly during this period). Filter with dry filter paper. If the filtrate is colored, add 2g of activated carbon, and place for 1h with occasional stirring. Then filter with dry filter paper. If it is still colored, replace the activated carbon and repeat the operation. 4.4.2.3 Test method
Take 50mL of the above test solution, place it in a 500mL conical flask, add 2mL of nitric acid solution and 10mL of silver nitrate standard solution (add more when the chloride content is high) and 5mL of nitrobenzene, shake vigorously until the silver chloride condenses, add 1mL of ammonium ferric sulfate solution, and titrate the excess silver nitrate to the end point with ammonium thiocyanate standard solution and keep it for 1min. At the same time, do a blank test in the same way. 4.4.2.4 Expression of analytical results
The mass percentage of chloride (in terms of NaCl) X is calculated according to formula (4): (V/- V)c × 0. 058 4 × 100 = X,
wherein V
m×200
(V, - V)c X 23. 36
The volume of 0.1 mal/L ammonium thiocyanate standard solution consumed in titrating the sample, mL; Y.
The volume of ammonium thiocyanate standard solution consumed in titrating the blank solution, mL; The actual concentration of the ammonium thiocyanate standard solution, mol/L; 0. 058 4
(４)
The mass of sodium chloride in grams equivalent to 1.00 mL of ammonium thiocyanate standard solution [c(NHCNS)=1.000 mal/L].
The mass of the sample + g.
4.4.2.5 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.3%. The arithmetic mean shall be taken as the determination result. 4.4.3 Determination of sulfate (as Na2SO4) content 4.4.3.1 Reagents and materials
a) Ammonia water;
b) Sodium hydroxide solution: 0.2g/L;
c) Hydrochloric acid solution: 1+99;
d) Ethanol: 95%;
e) Tetrahydroxybenzene disodium-potassium chloride mixed reagent: mix in equal amounts;f) Sulfuric acid standard solution: c(1/2H,SO,)=0.1mo1/L;g) Phenolic acid ethanol solution: 10g/L;
h) Sodium rhodamine indicator solution: weigh 0.1g of sodium rhodamine and dissolve it in 10mL of water (prepare and use immediately). i) Barium chloride standard solution: c(1/2BaCl,) = 0. 1 mol/L. Preparation: Weigh 12.25g of barium chloride, dissolve in 500mL of distilled water, transfer to a 1000mL volumetric flask, dilute to scale, and shake well. Calibration: Take 20mL of sulfuric acid standard solution, add 50mL of water, and neutralize with ammonia water until the bright yellow test paper shows an alkaline reaction, then titrate with barium chloride standard solution, use rose red sodium indicator solution as the liquid indicator, and the end point is the appearance of rose red spots on the filter paper that remain unchanged for 2 minutes. The concentration of barium chloride standard solution X, (mol/L) is calculated according to formula (5): Vc
Where: V——volume of sulfuric acid standard solution, mL; Vi——volume of barium chloride standard solution, mL; c—actual concentration of sulfuric acid standard solution, mol/L. $24
·(5)
4.4.3.2 Analysis steps
GB 17511. 1 - 1998
Pipette 25mL of the test solution and place it in a 250mL conical flask. Add 1 drop of phenolic alcohol indicator solution, add sodium hydroxide solution until it turns pink, then add hydrochloric acid solution until the pink disappears, then add 30mL of ethanol and 1.4g of tetrahydroxybenzoaldehyde disodium-potassium chlorofluoride mixed indicator, and shake well. After dissolution, titrate with barium chloride standard solution under constant shaking until the solution turns rose red. During the titration, use a light to illuminate and observe carefully from the side, and use rose red sodium indicator solution as an external indicator for comparison. At the same time, perform a blank test in the same way. 4.4.3.3 Expression of analysis results
Mass percentage of sulfate (in NazSO, X). Calculate according to formula (6): (V - Vi): c X 0.071
(V - V): c X 56.8
Wherein: V - volume of barium chloride standard solution consumed in titrating the sample solution, ml; V - volume of barium chloride standard solution consumed in titrating the blank solution, mL; c - actual concentration of the chloride standard solution, mol/L; 200
· (6)
0.071 - - sodium sulfate equivalent in grams to 1.00mL barium chloride standard titration solution Lc (1/2BaCl, = 1.000mol/L] Mass:
m-mass of the sample, g.
4.4.3.4 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4.4 Expression of analysis results
The sum of the mass percentage of drying loss, the mass percentage of chloride (in terms of NaCl) and the mass percentage of sulfate (in terms of Na.SO,) is calculated according to formula (7): X, =X+X++X
Mass percentage of drying loss, %;
Where; X—
X,——-Mass percentage of chloride, %; X. —Mass percentage of sulfate, %. 4.5 Determination of water-insoluble matter
4.5.1 Analysis steps
Weigh about 3g of sample, accurate to 0.01g, put it in a 500mL beaker, add 250mL of 50~~60℃ water to dissolve it, filter it with a No. 4 glass sand tower that has been dried to constant weight at 135℃±2℃, and wash it thoroughly with hot water until the washing liquid is colorless, and dry it in a constant temperature oven at 135℃±2℃ to constant weight.
4.5.2 Expression of analysis results
Mass percentage of water-insoluble matter X, calculated according to formula (8): Xg=㎡ × 100
Where: m:——the mass of water-insoluble matter after drying·g; m-—the mass of the sample, g.
4.5.3 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.05%, and the arithmetic mean shall be taken as the determination result. 4.6 Determination of low sulfonated secondary dye content
4.6.1 Reagents and materials
a) Methanol;
b) Ammonium acetate solution: 7.8g/L.
(8)
4.6.2 Instruments
Liquid chromatograph.
4.6.3 Preparation of test solution
GB 17511. 1—1998
Weigh 0.01g of the allure red sample, accurately to 0.0002g, add ammonium acetate solution to dissolve, and make up to 100mL, which is the test solution.
4.6.4 Preparation of standard solution
Weigh 0.01g of chlorhexidine sulfonic acid 3-hydroxyphenylphenol, accurately to 0.0002g. Dry it in a vacuum desiccator for 24h, dissolve it in 5mL of methanol, and add ammonium acetate solution to make up to 100mL. Weigh 0.01g of clesidi-nitrogen schiff salt to the nearest 0.0002g. Dry in a vacuum dryer for 24h, and add ammonium acetate solution to accurately make up to 100mL. Take 10mL of each of the above solutions and accurately make up to 100mL with ammonium acetate solution, as solution A and solution B. Then take 10.0mL, 5.0mL, 2.0mL, and 1.0mL of the above solution A and solution B, respectively, and make up to 100mL with ammonium acetate solution as standard solution. 4.6.5 Test conditions
Detector: visible light absorption detector (detection wavelength: 515nm); column filler: chemical bond type octadecyl silicon (5μm): column: stainless steel tube with an inner diameter of 4.6mm and a length of 15cm; column temperature: 40℃;
ammonium acetate solution: 7.8g/L;
mobile phase: a.
b. Methanol;
Concentration gradient: 50min linear concentration gradient from A:B (100:0) to A:B (0:100); flow rate: 1 mL/min.
4.6.6 Test method
Under the above given test conditions, take 20μL of the test solution and standard solution and directly perform liquid chromatography detection, then determine the peak height or peak area of each standard solution substance and prepare a standard curve. Determine the peak height or peak area of crissidine sulfonic acid azo 3-banphenol and crissidine azo Schaffner acid in the test solution, calculate the content of each substance according to the above standard curve, and then calculate their total value. 4.7 Determination of high sulfonated secondary dye content
4.7.1 Reagents and materials
Same as 4.6.1.
4.7.2 Instruments
Same as 4.6.2.
4.7.3 Preparation of test solution
Accurately pipette 20μL of the test solution prepared in 4.6.3 as the test solution. 4.7.4 Preparation of standard solution
Weigh 0.01 mol of crisidine sulfonic acid azo G salt and crisidine sulfonic acid azo R salt, respectively, to the nearest 0.0002 mol. Place in a vacuum dryer and dry for 24 hours, add ammonium acetate solution to accurately make up to 100mL, accurately pipette 10mL of each of the above solutions, and accurately make up to 100mL with ammonium acetate solution, respectively, as solution A and solution B. Then pipette 10.0mL, 5.0mL, 2.0mL, and 1.0mL of the above solution A and solution B, respectively, and accurately make up to 100mL with ammonium acetate solution as the standard solution. 4.7.5 Test conditions
Follow the test conditions specified in 4.6.5.
4.7.6 Test method
Take 20uL of the test solution and the standard solution respectively and directly perform liquid chromatography detection, then determine the peak height or peak area of each standard solution substance, make a standard curve, determine the peak height or peak area of crisidine sulfonic acid azo salt G and crisidine sulfonic acid azo salt R in the test solution, calculate the content of each substance according to the above standard curve, and then calculate the total value. 4.8 Determination of the content of 6-hydroxy-5-[(2-methoxy-5-methyl-4-sulfonylbenzene)azo}-8-(2-methoxy-5-methyl-4-sulfonylphenoxy)-2-naphthalenesulfonic acid disodium 126
salt
4.8.1 Reagents and materials
Same as 4.6.1.
4.8.2 Instruments
Same as 4.6.2.
4.8.3 Preparation of test solution
GB 17511. 1-- 1998
Accurately pipette 20uL of the test solution prepared in 4.6.3 as the test solution. 4.8.4 Preparation of standard solution
Weigh 0.01g of 6-hydroxy-5-[(2-methoxy-5-methyl-4-sulfonylbenzene)azo]-8-(2-methoxy-5-methyl-4-sulfonylphenoxy)-2-naphthalenesulfonic acid disodium salt, accurate to 0.0002g. Place in a vacuum dryer and dry for 24h, dissolve with ammonium acetate solution, accurately make up to 100mL, pipette 10ml of the solution. Add ammonium acetate solution to accurately make up to 100mL, and use this as solution A. Pipet 10.0mL, 5.0mL, 2.0mL1.0mL of solution A, and use ammonium acetate solution to accurately make up to 100mL. Use as standard solution. 4.8.5 Test conditions
According to the test conditions specified in 4.6.5.
4.8.6 Test method
Measure 20uL of the test solution and each standard solution and directly perform liquid chromatography detection, then determine the peak height or peak area of the substance in the standard solution, make a standard curve, determine the peak height or peak area of the substance in the test solution, and calculate the content of this substance based on the above standard curve. 4.9 Determination of sodium 6-hydroxy-2-naphthalenesulfonate content 4.9.1 Reagents and materials
Same as 4.6.1.
4.9.2 Instruments
Same as 4.6.2.
4.9.3 Preparation of test solution
Accurately pipette 20μL of the test solution prepared in 4.6.3 as the test solution. 4.9.4 Preparation of standard solution
Weigh 0.01g of sodium 6-hydroxy-2-naphthalenesulfonate to an accuracy of 0.0002B, place in a vacuum dryer and dry for 24h, dissolve with ammonium acetate solution, accurately make up to 100mL, take 10ml of the above solution and add ammonium acetate solution to accurately make up to 100mL as solution A. Take 3.0mL, 2.0mL and 1.0mL of solution A respectively, and make up to 100mL with ammonium acetate solution as standard solution. 4.9.5 Test conditions
Except that the detector is changed to an ultraviolet absorption detector (detection wavelength 290nm), all other test conditions are in accordance with the test conditions specified in 4.6.5. 4.9.6 Test method
Use 20 μL of test solution and each standard solution to directly perform liquid chromatography detection, then determine the peak height or peak area of sodium 6-hydroxy-2-naphthalenesulfonate in each standard solution, make a standard curve, determine the peak height or peak area of sodium 6-hydroxy-2-naphthalenesulfonate in the test solution, and calculate the content of this substance based on the above standard curve.
4.10 Determination of 4-amino-5-methoxy-2-methylbenzenesulfonic acid content 4.10.1 Reagents and materials
Same as 4.6.1.
4.10.2 Instruments
Same as 4.6.2.
4.10.3 Preparation of test solution
Accurately pipette 20 μL of the test solution prepared according to 4.6.3 as the test solution. 4.10.4 Preparation of standard solution
Weigh 0.01g 4-amino-5-methoxy-2-methylbenzenesulfonic acid to the nearest 0.0002 μg. Place in a vacuum desiccator and dry for 24 h. Dissolve in ammonium acetate solution to the nearest 100 mL. Take 10 mL of the above solution and add ammonium acetate solution to make up to 100 mL as solution A. Take 2.5 mL, 2.0 mL, and 1.0 mL of solution A respectively and make up to 100 mL with ammonium acetate solution as standard solution. 4.10.5 Test conditions
Follow the test conditions specified in 4.9.5.
4.10.6 Test method
Take 20μL of the test solution and each standard solution and directly perform liquid chromatography detection. Then determine the peak height or peak area of 4-amino-5-methoxy-2-methylbenzenesulfonic acid in each standard solution, make a standard curve, determine the peak height or peak area of 4-amino-5-methoxy-2-methylbenzenesulfonic acid in the test solution, and calculate the content of this substance based on the above standard curve. 4.11 Determination of the content of 6,6°-oxo-bis(2-naphthalenesulfonic acid) disodium salt 4.11.1 Reagents and materials
Same as 4.6.1.
4.11.2 Instruments
Same as 4.6.2.
4.11.3 Preparation of test solution
Accurately pipette 20L of the test solution prepared according to 4.6.3 as the test solution. 4.11.4 Preparation of standard solution
Weigh 0.01 g of 6,6°-oxo-bis(2-sulfonic acid) disodium salt to an accuracy of 0.0002g. Place in a vacuum dryer and dry for 24h, dissolve with ammonium acetate solution and accurately make up to 100mL. Take 10mL of the above solution, add ammonium acetate solution, and accurately make up to 100mL as solution A. Take 10.0mL, 5.0mL, 2.0mL, and 1.0mL of solution A respectively, and accurately make up to 100mL with ammonium acetate solution as standard push solution. 4.11.5 Test conditions
According to the test conditions specified in 4.9.5.
4.11.6 Test method
Use 20ul test solution and each standard solution to directly perform liquid chromatography detection, then determine the peak height or peak area of 6,6°-oxo-bis(2-naphthosulfonic acid) disodium salt in each standard solution, prepare a standard curve, determine the peak height or peak area of 6,6°-oxo-bis(2-sulfonic acid) disodium salt in the test solution, and calculate the content of this substance according to the above standard curve. 4.12 Determination of the total content of unsulfonated aromatic primary amines (calculated as aniline) 4.12.1 Reagents and materials
a) Methanol;
b) Chloroform;
c) Aniline;
d) Sodium hydroxide solution: 40g/L
e) Sulfuric acid solution: 0.15+100;
f) Sodium dihydrogen phosphate solution: 15.2g/L, Preparation: Weigh 15.2g of sodium dihydrogen phosphate and dissolve it in water, add about 0.1ml of sulfuric acid solution (1+4), place it in a 1000mL volumetric flask, and dilute to the scale.
g) Diatomaceous earth for chromatography.
4.12.2 Instruments
Liquid chromatograph.
4.12.3 Preparation of test solution
Weigh 1.0g of the allure red sample to an accuracy of 0.001g, add 10mL of water and 2 drops of sodium hydroxide solution, and heat in a water bath to dissolve to obtain a sample solution.
Put chromatographic diatomaceous earth in a glass tube with an inner diameter of about 2.5cm to make a 10cm high chromatographic diatomaceous earth layer as an absorption column, add the sample solution into the column and let it flow down, washing the container used to prepare the sample solution with 2mL of water each time for a total of three times. Pour 528
of each washing solution into the absorption column.
GB 17511. 1-1998
Add 25mL of chloroform to the column and collect the outflowing liquid into a 200mL round-bottom flask. Repeat the above operation three times with 25mL of chloroform each time, and add 5mL of sulfuric acid to the collected liquid. Concentrate the liquid with a rotary evaporator at 45℃, and remove the chloroform remaining in the flask with a nitrogen stream. Add 0.1mL of sodium dihydrogen phosphate solution and a small amount of water to the residue, and make it up to 5mL accurately. This solution is used as the test solution.
4.12.4 Preparation of standard solution
Weigh 1.0g of aniline, accurate to 0.001g. Dissolve it in methanol and make it up to 100mL accurately. Absorb 10mL, add methanol to the solution and make it up to 100mL accurately. This solution is solution A. Take 10.0mL, 5.0mL, 2.0mL and 1.0mL of solution A respectively, add water to make up to 100mL, and use this as the initial standard solution. Take each initial standard solution, add 10mL of water and 2 drops of sodium hydroxide solution respectively, and then add the above solution to the absorption column to make it flow down, and operate according to the provisions of the test solution preparation process to prepare each standard solution. 4.12.5 Test conditions
According to the test conditions specified in 4.9.5.
4.12.6 Test method
Accurately take 20uL of the test solution and each standard solution and directly perform liquid chromatography detection, then determine the peak height or peak area of aniline in each standard solution, prepare a standard curve, determine the peak height or area of the aniline peak in the test solution and the peak that appears within 30 minutes after the aniline peak appears, and calculate the total aniline content according to the above standard curve. 4.13 Determination of arsenic content
4.13.1 Reagents and materials
a) Nitric acid;
b) Sulfuric acid solution: 1→1;
c) Nitric acid-perchloric acid mixed solution: 3+1; d) Arsenic standard solution: 0.001mgAs/mL. Take 1mL of the standard solution containing 0.1mgAs/mL in a 100mL volumetric flask and dilute to the mark.
4.13.2 Instruments and equipment
Apparatus according to the arsenic spot method in GB/T8450.
4.13.3 Analysis steps
Weigh 1.0g of the sample, accurate to 0.01g. Place in a round-bottom flask, add 1.5mL of nitric acid and 5mL of sulfuric acid, heat over low heat to drive out nitrogen dioxide gas, and stop heating when the solution turns brown. After cooling, add 5 mL of nitric acid-perchloric acid mixture and heat with strong fire until the solution is transparent, colorless or slightly yellow. If it is still opaque, add about 5 mL of nitric acid-perchloric acid mixture after cooling, continue heating until the solution is clear, colorless or slightly yellow and produces white smoke, then stop heating. After cooling, add 5 mL of water and heat to boiling, remove the residual nitric acid-perchloric acid (add water and boil once more if necessary), continue heating until white smoke is produced, keep for 10 minutes, cool and move to a 100 mL conical flask. The following shall be carried out in accordance with the provisions of 2.4 in GB/T8450-1987. 4.14 Determination of heavy metal content
4.14.1 Reagents and materials
a) Sulfuric acid;
b) Hydrochloric acid:
c) Hydrochloric acid solution: 1+3;
d) Acetic acid solution: 1+3;
e) Ammonia solution: 1+2;
f) Sodium sulfide solution: 100g/L;
g) Lead standard solution: 10mL of lead standard solution containing 0.1mgPb/mL is taken into a 100mL volumetric flask and diluted to the scale.
4.14.2 Preparation of sample solution
GB 17511.1—1998
Weigh 2.5g of the sample, accurate to 0.01. Place in a platinum (or quartz, porcelain) container, add a small amount of sulfuric acid to moisten it, slowly burn it, try to make it almost completely ash at low temperature, then add 1mL of sulfuric acid, gradually heat until sulfuric acid vapor almost stops. Place in an electric furnace, burn at 450℃～550℃ until it is ash, then cool. Add 3mL of hydrochloric acid and shake well, then add 7mL of water and shake well, filter with quantitative analysis filter paper (No. 5C). Wash the residue on the filter paper with 5mL of hydrochloric acid solution and 5mL of water, combine the washing liquid and the filtrate, add water to make it 50nL, as the sample solution.
Use the same method without adding sample to prepare a blank test solution. 4.14.3 Preparation of test solution
Measure 20 mL of the test solution, place it in a Nessler colorimetric tube, add 1 drop of phenolic acid test solution, add ammonia solution until the solution turns red, then add 2 mL of acetic acid solution, filter if necessary, wash the filter paper with water, and add water to make it up to 50 mL as the test solution. 4.14.4 Preparation of comparison solution
Measure 20 mL of blank test solution, place it in a Nessler colorimetric tube, add 2.0 mL of lead standard solution and 1 drop of phenolic acid indicator solution, and prepare it in the same way as the test solution as the comparison solution.
4.14.5 Test method
Add 2 drops of sodium sulfide solution to the test solution and the comparison solution respectively, shake it, and after standing for 5 minutes, the color of the test solution shall not be darker than that of the comparison solution.
4.15 Determination of lead content
4.15.1 Reagents and materialswww.bzxz.net
Same as 4.14.1.
4.15.2 Preparation of test solution
Take 10mL of the sample solution prepared in 4.14.2 as the test solution. 4.15.3 Preparation of comparison solution
Take 1.0mL of lead standard solution and add dilute hydrochloric acid solution to make up to 20mL as the comparison solution. 4.15.4 Test method
Add 2 drops of sodium sulfide solution to the test solution and the comparison solution respectively, shake and place for 5 minutes. The color of the test solution shall not be darker than that of the comparison solution.
5 Inspection rules
5.1 Food additive Allure Red shall be inspected by the product quality inspection department of the production unit. The production unit shall ensure that the quality of all food additive Allure Red shipped from the factory meets the requirements of this standard and has a quality certificate in a certain format. 5.2 The user unit may inspect the quality of the food additive Allure Red received in accordance with the inspection rules and test methods specified in this standard to check whether its quality indicators meet the requirements of this standard. 5.3 Food additive Allura Red is a batch of one production batch number. 5.4 Sampling should be done by selecting 10% of the total number of boxes (each box is 10×0.5kg) of each batch of products, and then selecting 10% of the bottles from the selected boxes. Take out no less than 50 samples from the center of each bottle from the selected bottles. Be careful when sampling to prevent foreign matter from falling into the product. Mix the sample quickly and take about 100g from it, and put it in two clean, dry ground glass bottles, and seal them with paraffin. Mark the manufacturer name, product name, batch number, and production date. One bottle is for inspection and one bottle is kept. 5.5 If one of the indicators does not meet the requirements of this standard during the inspection, samples should be selected from twice the amount of packaging for re-inspection. If one of the indicators still does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6 Marking, packaging, transportation, storage
6.1 The packaging box should have obvious markings, including: "Food Additives\, product name, trademark, manufacturer name, manufacturer address, specifications, batch number, production date, production license number, number of bottles. 33
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.