Some standard content:
GB17512.2—1998
This standard is equivalent to the "Japanese Food Additives Standard (1992) Sixth Edition" and is formulated based on the "Edible Red No. 3 Aluminum Lake (Erythrosine Aluminum Lake)" standard in the book.
The main differences between this standard and the Japanese standard are as follows: 1 The determination method of chloride (in terms of NaCl) and sulfate (in terms of NazSO.) in this standard is chemical titration, while the Japanese standard uses ion chromatography.
2 The determination method of secondary dye content in this standard adopts the determination method in WHO/FAO, and the index is ≤1.5%. 3 The determination of arsenic content adopts GB/T8450-1987 "Determination of Arsenic in Food Additives", which refers to The standard is ≤0.0003% (As), and the Japanese standard is ≤0.0004% (As20). This standard is proposed by the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the former dye standardization technical unit of the 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 Health Bureau. The main drafters of this standard are Qiu Yumei, Liu Jing, Ding Deyi, Shi Huaijiong, Qian Kai, and Zhou Yanqin. This standard is entrusted to the former dye standardization technical unit of the Ministry of Chemical Industry for interpretation. 52
1 Scope
National Standard of the People's Republic of China
Food Additives
Erythrosine Aluminum LakeWww.bzxZ.net
Food additive
Erythrosine aluminum lake
GB 17512. 2 -1998
This standard specifies the requirements, test methods, inspection rules, marking, packaging, transportation and storage of the food additive erythrosine aluminum lake. This standard applies to the pigment lake generated by the reaction of the food additive erythrosine and aluminum hydroxide. This product can be added to food as a colorant.
Molecular formula: C2H.I,Os
Relative molecular mass: 835.90 (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. All parties using this standard should explore the possibility of using the latest version of the following standards. : Preparation of standard push solution for titration analysis (volume analysis) of chemical reagents GB/T 601—1988
Chemical reagents Preparation of standard solutions for determination of impurities GB/T 602--1988
GB/T 603--1988
Chemical reagents Preparation of preparations and products used in test methods GB/T6682—1992 Specifications and test methods for water used in analytical laboratories (neqISO3696:1987) GB17512.1—1998 Food additive Erythrosine 3 Requirements
3.1 Appearance: red powder.
3.2 Food additive Erythrosine aluminum lake should meet the requirements of Table 1. Table 1 Requirements
Content (as color acid)
Loss on drying
Insoluble matter in hydrochloric acid and ammonia water
Chloride (as NaCl)
And sulfate (as Na,SO,)
Subsidiary dye
Arsenic (As)
Heavy metal (as Pb)
Barium (Ba)
Sodium iodide
Approved by the State Administration of Quality and Technical Supervision on October 19, 1998
Implementation on April 1, 1999
4 Test method
GB 17512. 2—1998
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and Grade 3 water specified in GB/T6682. 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
4.2.1 Reagents and materials
a) Sulfuric acid:
b) Sodium hydroxide solution: 90g/L;
) Ammonium acetate solution: 1.5g/L;
d) Hydrochloric acid solution: 1+3.
4.2.2 Instruments and equipment
Spectrophotometer.
4.2.3 Test method
4.2.3.1 Weigh about 0.1g of sample, add 5mL of sulfuric acid, shake and heat in a water bath from time to time, and it will turn light brown-orange after about 5min. After cooling, take 2~3 drops of the upper clear liquid, add 5mL of water, and produce an orange-red precipitate. 4.2.3.2 Weigh about 0.1B of sample, add 5mL of sodium hydroxide solution, heat and dissolve in a water bath, add ammonium acetate solution to 100ml. Then absorb 2mL. Use ammonium acetate solution to 100mL. The maximum absorption wavelength of the solution should be 526nm±2nm. 4.2.3.3 Weigh 0.1g of sample, add 10mL of hydrochloric acid solution, heat in a water bath for 5min, shake to dissolve, add 0.5g of activated carbon, shake well and filter. The solution is clear and red. Cool and neutralize with sodium hydroxide until a red colloidal precipitate gradually forms. 4.3 Determination of the content of erythrosin aluminum lake Spectrophotometric colorimetric method 4.3.1 Summary of the method
After the sample is treated, its absorbance is measured at the maximum absorption wavelength by a spectrophotometer, and then the content of the sample is calculated. 4.3.2 Reagents and materials
a) Sodium hydroxide solution: 4 g/L;
b) Ammonium acetate solution: 1.5 g/L
4.3.3 Instruments and equipment
a) Spectrophotometer;
b) Colorimetric III: 10 mm.
4.3.4 Analysis steps
Accurately weigh 0.1 g of erythrosin aluminum lake, put it into a 100 mL beaker, add 50 ml of sodium hydroxide solution to dissolve it, and transfer it to a 500 mL volumetric flask. Then wash the beaker with ammonium acetate solution, add the washing solution into the volumetric flask, add ammonium acetate solution, and accurately make up to 500 mL as the sample solution. Then accurately measure 10-20 mL of the sample solution, add ammonium acetate solution, and accurately make up to 200 mL as the test solution. Measure the absorbance A on a spectrophotometer at a wavelength of 526 nm ± 2 nm using 10 mm colorimetric blood. 4.3.5 Expression of analysis results
The mass percentage content X of erythrosine aluminum lake is calculated according to formula (1): AX 500 × 200 × 0.931
0.111 × m. V × 1 000
Wherein: A-absorbance;
Sample volume, mg:
V——Sample solution used to prepare the test solution, mL: X 100
0.111——Conversion factor for spectrophotometry; GB 17512.2-1998
0.931-Conversion factor for erythrosine acid and pigment (monohydrate of sodium salt). 4.4 Determination of loss on drying
According to 4.4.1 of GB17512.1-1998.
4.5 Determination of insoluble matter in hydrochloric acid and ammonia water 4.5.1 Reagents and materials
a) Hydrochloric acid:
b) Hydrochloric acid solution: 1+3;
c) Ammonia solution: 4+96;
d) Silver nitrate solution: c(AgNO,)=0.1mol/L 4.5.2 Analysis steps
Weigh 2g of sample, accurate to 0.01g, put it in a 600mL beaker, add 20mL of water and 20mL of concentrated hydrochloric acid, stir thoroughly, then add 300mL of hot water and stir well, cover the surface with blood, heat in a water bath at 70~～80℃ for 30min, and let cool. Filter with G4 glass sand that has been dried to constant weight at 135℃±2℃, rinse the insoluble matter in the beaker into the crucible with water until the washing liquid is colorless, wash with 100mL ammonia solution, then wash with 10mL hydrochloric acid solution, and then wash with water until there is no white precipitation when detected by silver nitrate solution, and then put it into a constant temperature oven at 135℃:±2℃ to dry to constant weight.
4.5.3 Expression of analysis results
The mass percentage of insoluble matter in hydrochloric acid and ammonia water is X. Calculate according to formula (2): m×100
Where: ml mass of insoluble matter after drying + g, m mass of sample; g.
4.5.4 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 The determination of chloride (as NaCl) and sulfate (as Na, SO,) content shall be in accordance with 4.4.2~4.4.3 of GB17512.1-1998. The sum of the mass percentage of chloride and sulfate shall not exceed 2.0%. 4.7 Determination of secondary dye content
4.7.1 Method Summary
Use paper chromatography to separate and elute the components, and then quantify them by spectrophotometry. 4.7.2 Reagents and Materials
a) n-Butanol;
b) Ethanol;
c) Ammonia solution: 4+96;
d) Sodium hydroxide solution: 100g/L;
e) Sodium bicarbonate solution: 4g/L;
f) Acetone solution; 1+1.
: 4.7.3 Instruments and equipment
a) Spectrophotometer:
b) Chromatographic filter paper: No. 1 medium speed, 150mm×250mm; c) Chromatographic cylinder: $240mm×300mm
d) Micro-injector: 100uL,
e) Nessler colorimetric tube: 50mL, with ground stopper. · (2)
4.7.4 Analysis steps
4.7.4.1 Paper chromatography conditions
GB 17512. 2- 1998
Developing solvent: n-butanol + ethanol + ammonia solution = 6 + 2 + 3; Temperature: 20~25°C.
4.7.4.2 Preparation of sample eluate
Weigh 1g of sample, accurate to 0.01g, place in a beaker, add appropriate amount of water and 50mL of sodium hydroxide solution, heat to 80-90℃, stir to dissolve.
Transfer to a 100mL volumetric flask, dilute to scale, shake well, draw 200μL with a microinjector, and evenly apply it on a baseline 25mm away from the bottom edge of the filter paper in a straight line so that the width of the solution on the filter paper does not exceed 5mm and the length is 130mm. Blow dry with a hair dryer. Place the filter paper in the chromatography cylinder for development, immerse the bottom edge of the filter paper 10mm below the liquid surface of the developing agent, and wait until the front line of the developing agent rises to 150mrn or until the secondary dye is separated satisfactorily. Take out the chromatography filter paper and blow dry with a hair dryer with cold air. At the same time, develop with blank filter paper under the same conditions [the blank filter paper must be cut from the same part of the filter paper (600mmX600 mm) as the filter paper used for developing the test solution]. Cut each secondary dye and the filter paper corresponding to each secondary dye on the blank filter paper to the same size, and cut into thin strips of about 5mmX15mm, and place them in 50mL Nessler colorimetric tubes, accurately add 5mL of acetone solution to each, shake for 3 to 5 minutes, and then accurately add 20mL of sodium bicarbonate solution and shake thoroughly. Filter the extracts naturally in No. 3 glass sand core funnels, and the filtrate must be clear and free of suspended matter. At the maximum absorption wavelength of each secondary dye, use a 50mm colorimetric dish to measure the absorbance on a spectrophotometer. Use a mixture of 5mL acetone solution and 20mL sodium bicarbonate solution as a reference solution. 4.7.4.3 Preparation of standard eluate
Accurately pipette 6mL of the above 1% sample solution into a 100mL volumetric flask, dilute to the mark, and shake. Use a microinjector to pipette 200μl. Evenly apply it on a baseline 25mm from the bottom edge of the filter paper, and blow it dry with cold air. Place the filter paper in the chromatography cylinder and develop it. When the front line of the developing agent rises only 40mm, take it out and blow it dry. Cut off all the dye parts and perform the extraction operation as before. Use a 100mm thick colorimetric III to measure the absorbance at the maximum absorption wavelength.
At the same time, develop it with a blank filter paper under the same conditions, and measure the absorbance of the extract after the same operation. 4.7.4.4 Expression of analysis results
The mass percentage content X of the secondary dye is calculated according to formula (3): (A, - b)) + + (A, - b.)
×6×s
Wherein: A,,*.A.The absorbance of each secondary dye extract calculated at a light path length of 50 mm: by.....,b..
The absorbance of each secondary dye reference blank extract calculated at a light path length of 50 mm: A The absorbance of the standard extract calculated at a light path length of 10 mm; The absorbance of the standard reference blank sample calculated at a light path length of 10 mm; b,
The ratio converted to a light path length of 10 mm;
6—the reference concentration of the standard extract based on the 1% sample solution, %S——the total content of the sample.
4.7.4.5 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. 4.8 Determination of arsenic content
According to 4.7 of GB17512.1-1998.
4.9 Determination of heavy metal content
4.9.1 Reagents and materials
a) Sulfuric acid;
*++++++++( 3 )
b) Hydrochloric acid;
c) Nitric acid;
d) Hydrochloric acid solution: 1+3;
e) Ammonium acetate solution: 1+9;
f) Sodium sulfide solution: 100g/L
GB 17512. 2 -1998
g) Lead standard solution: 0.01mgPb/mL. Take 10mL of the lead standard solution containing 0.1mgPb/mL in a 100mL volumetric flask and dilute to the mark.
4.9.2 Analysis steps
Weigh 5g of the sample, accurate to 0.01g. Put it in a quartz or porcelain crucible, add a little sulfuric acid to moisten it, slowly burn it, and try to ash it at low temperature, then cool it down. Add 1mL of sulfuric acid and slowly heat it until sulfuric acid vapor almost stops. Put it in an electric furnace and burn it at 450~55a℃ for 3h, then cool it down. Add 5mL of hydrochloric acid and 1mL of nitric acid, crush it thoroughly, and evaporate it on a water bath. Add 5mL of hydrochloric acid, crush it thoroughly, and evaporate it on a water bath. Add 10mL of hydrochloric acid solution, heat it to dissolve, and after cooling, filter it with quantitative analysis filter paper (No. 5C). Wash the container and the residue on the filter paper with 5mL of hydrochloric acid solution and a small amount of water, combine the washing liquid and the filtrate, and add water to make it 50mL as the sample solution. Perform the same operation without using the sample as the blank test solution. Measure 20mL of the sample solution, add ammonium acetate solution, adjust to a pH value of about 4, and add water to make it 50mL as the test solution. Also measure 20mL of the blank test solution and 2.0mL of the lead standard solution, and perform the same operation as the sample to make a comparative solution. After adding 2 drops of sodium sulfide test solution to each of the two solutions, shake well, and let stand for 5 minutes. The color of the test solution should not be darker than that of the comparative solution. 4.10 Determination of lock content
4.10.1 Reagents and materials
a) Sulfuric acid;
b) Sulfuric acid solution: 1+19;
c) Hydrochloric acid solution: 1+3.
4.10.2 Analysis steps
Weigh about 1g of the sample, accurate to 0.01g, put it in a platinum (right imperial or porcelain), add a small amount of sulfuric acid to moisten it, slowly heat it, try to make it almost completely ash at low temperature, let it cool, add 1mL of sulfuric acid, slowly heat until almost no sulfuric acid vapor is generated, put it in an electric furnace, and burn it at 450550℃ for 3h. After cooling, add more than 5% anhydrous sodium carbonate and mix thoroughly, cover and heat to melt. Continue heating for 10min, cool, add 20mL of water, heat on a water bath to dissolve the molten material. After cooling, filter, wash the residue on the filter paper with water until the washing liquid does not react with sulfate. Then transfer the residue on the paper and the filter paper to a beaker, add 30mL of hydrochloric acid solution, shake thoroughly and boil. After cooling, filter, wash the residue on the filter paper with 10mL of water, combine the washing liquid and the filtrate, and evaporate to dryness on a water bath. Add 5mL of water to dissolve the residue, filter if necessary, add water to make it 10mL, add 0.1mL of hydrochloric acid solution, mix thoroughly, add 1mL of sulfuric acid solution and mix, let stand for 10 minutes, no turbidity.
4.11 Determination of sodium iodide content
4.11.1 Reagents and materials
Silver nitrate standard solution: c(AgNO.)=0.001mol/L. 4.11.2 Instruments and equipment
a) Digital millivoltmeter:
b) Iodide ion selective electrode:
c) Reference electrode;
d) Electromagnetic stirrer.
4.11.3 Preparation of test solution
Weigh 2.0g of sample, accurate to 0.0002g, place in a beaker, add 75ml of accurately measured water, stir with an electromagnetic stirrer for about 30 minutes, filter with dry filter paper in a glass sand crucible funnel, and use the filtrate as the test solution. The test method is in accordance with 4.9.4 of GB17512.1--1998. 557
4.11.4 Expression of analysis results
GB17512.2-1998
The percentage content of sodium iodide by mass is X. Calculate according to formula (4): X = V × 0:001 5 × 100
Where: m——mass of the sample, g,
V-—volume of the silver nitrate standard solution consumed in the titration of the sample, mL: (4)
0.0015—with 1.00 mol/L silver nitrate standard titration solution [c (AgNO.) = 1.000mol/L is equivalent to the mass of sodium iodide expressed in grams.
5 Inspection rules
5.1 The food additive erythrosine aluminum lake shall be inspected by the product quality inspection department of the production unit. The production unit shall ensure that the quality of all food additives erythrosine aluminum lakes sold meets the requirements of this standard and have a quality certificate in a certain format. 5.2 The user unit may inspect the quality of the food additive erythrosine aluminum lake 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 erythrosine aluminum lake is a batch of products with one production batch number. 5.4 Sampling should select 10% of the total number of boxes (each box is 10×0.15kg) of each batch of products, and then select 10% of the bottles from the selected boxes. From the selected bottles, take out no less than 50 samples at the center of each bottle. Be careful when sampling to prevent foreign impurities from falling into the product. After mixing the sample quickly, take about 100g from it and put it into two clean, dry ground glass bottles, seal them with paraffin, and mark the manufacturer's name, product name, batch number, and production date. One bottle is for inspection and one bottle is for storage. 5.5 If one indicator 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 the re-inspection result 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, production address, specifications, batch number, production date, production license number, number of bottles. 6.2 Each bottle of product leaving the factory should be accompanied by a quality certificate, including: manufacturer name, product name, batch number, production date, net content, instructions for use, proof that the product quality complies with this standard and standard number. 6.3 Food additive erythrosine aluminum lake is packed in polyethylene plastic bottles, each bottle is 0.15kg, and every 10 bottles are sealed in a carton. 6.4 It must be protected from rain, moisture and sunlight during transportation, and should be stored in a dry and cool warehouse. 6.5 This product must not be mixed, transported or stacked together with other toxic, harmful or other substances during storage and transportation. 6.6 The shelf life of this product is five years from the date of production. If it is overdue, re-inspect whether it meets the requirements of this standard, and it can still be used if it is qualified. 558
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