Some standard content:
GB 16313—1996
This standard is equivalent to the 1983 edition III of the Food Chemicals Code (FCC) of the United States. The product properties, description, identification, content, salt, heavy metals, lead, loss on drying, and specific rotation all adopt the FCC standard, and the pH value adopts the United States Pharmacopoeia (USP) 23rd edition standard. This standard is basically consistent with the current international standards.
The specific test methods of this standard basically adopt the current national standards. When there is no or it is impossible to adopt the national standards, the methods specified by the US FCC are adopted.
This standard is proposed by the State Drug Administration. This standard is technically managed by China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. The responsible drafting unit of this standard: Jiangsu Jiangshan Pharmaceutical Co., Ltd. The main drafters of this standard: Ji Weiwen, Xi Chuanlin, Shen Yan. After investigation, the FCC 1994 edition of this product has not been modified. 289
1 Scope
National Standard of the People's Republic of China
Ascorbic acid
Food additive
-Sodium ascorbate
GB 163131996wwW.bzxz.Net
This standard specifies the technical requirements, test methods, inspection rules, packaging and labeling, transportation and storage requirements of food additive sodium ascorbate.
This standard applies to sodium ascorbate made from ascorbic acid and sodium salt as raw materials, which is used as a nutritional enhancer and antioxidant in the food industry.
2 Cited 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 are subject to revision, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB613-88 General determination method for specific rotation of chemical reagents GB6284--86 General method for determination of moisture content in chemical products Gravimetric method GB8449--87 Determination method for lead in food additives GB8450-87 Determination method for arsenic in food additives "Pharmacopoeia of the People's Republic of China" 1995 edition (Part II) 3 Chemical name, molecular formula, structural formula, molecular weight Chemical name: sodium ascorbate
sodium ascorbate
Molecular formula: CH,NaO.
Structural formula:
ONa OH
HOCH,C
Molecular weight: 198.11 (according to the international atomic weight of 1987) 4 Technical requirements
4.1 Properties
This product is a white to slightly yellow crystalline solid. 1g of this product can be dissolved in 2mL of water. 4.2 Items and indicators
Approved by the State Bureau of Technical Supervision on May 21, 1996, 290
Implementation on December 1, 1996
Content (as CH4, NaO2) (as dry product), % Arsenic (as As), %
Heavy metals, %
Lead (Pb), %
Loss on drying, %
Specific rotation [α (as dry product)
5 Test method
GB 16313-1996
99. 0~101. 0
+103°～+108°
The reagents used in this standard are analytical reagents, water is distilled water or water of corresponding purity, unspecified solutions are aqueous solutions, and the instruments and equipment are general laboratory instruments and equipment. Each batch of products should be fully inspected according to the technical characteristics specified in this standard. 5.1 Identification
5.1.1 Principle
The ascorbic acid part in this product has a diene alcohol structure, has strong reducing properties, and has the properties of sugars. 5.1.2 Reagents and solutions
5.1.2.1 Alkaline copper tartrate test solution
1) Take 6.93g of copper sulfate crystals and add water to dissolve it into 100mL. 2) Take 34.6g of potassium sodium tartrate crystals and 10g of sodium hydroxide and add water to dissolve it into 100mL. When using, mix 1) and 2) in equal amounts to obtain. 5.1.2.2 Methylene blue test solution
0.5% (W/V) ethanol solution.
5.1.2.3 Dilute hydrochloric acid
Take 9ml of hydrochloric acid (GB622), add water to dilute to 1000ml, and you will get 5.1.2.4 Uranium oxyacetate zinc test solution
Take 10g of uranium oxyacetate, add 5mL of glacial acetic acid and 50ml of water, and heat slightly to dissolve it. Take another 30g of zinc acetate, add 3mL of glacial acetic acid and 30mL of water, and heat slightly to dissolve it. Mix the two liquids, cool them, and filter them to get it. 5.1.2.5 Trichloroacetic acid test solution
Take 6g of trichloroacetic acid, add 25mL of chloroform to dissolve it, then add 0.5ml of 30% hydrogen peroxide solution, shake well, and you will get it. 5.1.3 Identification method
5.1.3.11:50 of this solution can reduce alkaline copper tartrate test solution at 25℃, and it is faster when heated. 5.1.3.2 Acidify 2 mL of 1:50 sample solution with 0.5 ml of 0.1 mol/1. hydrochloric acid, add 4 drops of methylene blue test solution, warm at 40°C, and the dark blue color fades within 3 minutes.
5.1.3.3 Dissolve 15 mg of sample with 15 ml of 1:20 trichloroacetic acid solution, add about 200 mg of activated carbon, shake vigorously for 1 minute, filter with a small chrysanthemum filter paper, and filter again until clear if necessary. Add a drop of pyrrolidone to 5 mL of filtrate, stir slowly until dissolved, and then heat in a 50°C water bath to produce blue.
5.1.3.4 The characteristic reaction of sodium salt is shown in Appendix 14 of the 1995 edition (Part II) of the Pharmacopoeia of the People's Republic of China. 5.2 Content determination
5.2.1 Principle
The sample undergoes a redox reaction with the iodine titration solution, and the titration end point is determined by the color of the iodine titration solution. 291
5.2.2 Reagents and solutions
5.2.2. 1 Iodine (GB 675).
GB16313--1996
5.2.2.2 Iodine standard titration solution: 0.1mol/L iodine standard titration solution is prepared according to page 187 of Appendix to the 1995 edition (Part II) of the Pharmacopoeia of the People's Republic of China. 5.2.2.3 Dilute sulfuric acid
Take 57ml of sulfuric acid (GB625), slowly inject it into an appropriate amount of water, cool it to room temperature, dilute it to 1000ml with water, and shake it well. 5.2.2.4 Starch indicator solution
Prepare it according to page 179 of Appendix to the 1995 edition (Part II) of the Pharmacopoeia of the People's Republic of China. 5.2.3 Determination method
Accurately weigh about 400 mg of the product dried with phosphorus pentoxide for 24 h, accurate to 0.0002 g, and dissolve it in a mixture of 100 mL of freshly boiled cold distilled water and 25 mL of dilute sulfuric acid test solution. Immediately titrate with 0.1 mol/L iodine solution. When near the end point, add 3 mL of starch indicator solution until the solution turns blue and does not fade within 30 s (each 1 mL of 0.1 mol/L iodine solution is equivalent to 9.905 mg of sodium ascorbate). 5.2.3.1 Expression of analytical results
The sodium ascorbate content X is expressed as mass percentage and calculated according to formula (1): X = V:F × 0. 009.905 × 100
Wherein: V-→volume of iodine standard titration solution consumed by the sample, mL; measured concentration of titration solution (mal/L)
F-converted value of concentration of iodine standard titration solution, F=specified concentration of arc titration solution (mol/L)
mi-—mass of sample, g;
0.009905-——mass of sodium ascorbate (CH,NaO,) in grams equivalent to 1.00mL iodine standard titration solution [c(1/212)==0.1mol/L].
5.2.4 Allowable error
The relative deviation of the results of two parallel determinations in this method shall not exceed 0.3%. 5.3 Determination of arsenic salts
5.3.1 Reagents and solutions
5.3.1.1 Hydrochloric acid (GB622).
5.3.1.2 Arsenic standard solution
Prepare according to GB8450. 1.0 mL of this solution is equivalent to 1.0 μg of the monument. 5.3.2 Determination method
Take 3 g of sample (accurate to 0.002 g) and determine it by the GB8450 arsenic spot method. 5.4 Determination of heavy metals
5.4.1 Reagents and solutions
5.4.1.1 Acetate buffer solution of pH 3.5
Prepare according to page 175 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.4.1.2 Thioacetamide test solution
Prepare according to page 170 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.4.1.3 Lead standard solution
Prepare according to page 54 of Appendix to the 1995 edition (Part II) of the Pharmacopoeia of the People's Republic of China. .1
5.4.2 Determination method
5.4.2.1. Tube A: Pipette 2.0 ml of lead standard solution into a 50 ml Nessler colorimetric tube, add water to 25 ml, mix well, add 2 ml of pH 3.5 acetate buffer, mix well, and set aside.
5.4.2.2. Tube B: Take a Nessler colorimetric tube that matches tube A, weigh 1.0 g of sample into the Nessler colorimetric tube, add water to 25 ml, mix well, add 2 ml of pH 3.5 acetate buffer, mix well, and set aside. 292
GB16313-1996
5.4.2.3. Add 2 ml of thioacetamide test solution into both tubes, mix well, place in a dark place for 2 min, and observe on a white background, from top to bottom. The color of tube B shall not be darker than that of tube A. The first and second methods of the heavy metal inspection method in the Appendix 54-55 of the 1995 edition of the Pharmacopoeia of the People's Republic of China (Part II) were used. The test results were completely consistent. The first method was used as the inspection method and the second method was used as the arbitration method. 5.5 Determination of lead
5.5.1 Reagents and solutions
5.5.1.1 Diammonium hydrogen citrate (HG3-1465): 50% solution prepared according to GB8449-87.
5.5.1.2 Potassium cyanide: 10% solution
5.5.1.3 Diphenylthiobarb (dithiol)
Prepare according to GB8449-87.
5.5.1.4 Lead standard solution
Accurately weigh 0.1598g of high-purity lead nitrate (HG3-1309), add 10mL of 1% nitric acid, dissolve and transfer quantitatively into a 100mL volumetric flask, and dilute to the mark with water. 1mL of this solution is equivalent to 1mg of lead. Dilute it 100 times with water before use so that 1mL is equivalent to 10g of lead. 5.5.1.51% nitric acid
Take 1mL of nitric acid (GB626) and dilute to 100mL with water. 5.5.2 Determination method
Weigh 1g of sample and 2mL of lead limit standard solution (equivalent to 20μg of lead), respectively, and place them in 125mL separatory funnels, and add 1% nitric acid to 20mL each.
Add 1mL 50% ammonium citrate solution, 1mL 20% hydroxylamine hydrochloride solution and 2 drops of phenol red indicator solution to the sample solution and the lead limit standard solution, adjust to red with ammonia water (1+1), then add 2mL 10% potassium cyanide solution to each solution, mix well, add 5.0mL disulfide working solution, shake vigorously for 1min, let stand and separate, and then compare colors visually. The color of the trifluoromethane layer of the sample solution shall not be darker than that of the trifluoromethane layer of the lead limit standard solution.
5.6 Loss on Drying
5.6.1 Instrument
Oven, the sensitivity can be controlled at ±2℃, equipped with a thermometer, the depth of the thermometer inserted into the oven should make the mercury ball and the sample to be tested on the same level.
5.6.2 Determination method
Weigh about 3g of the sample, place it in a flat weighing bottle that has been dried to constant weight under the same conditions as the sample, weigh it accurately, and dry it to constant weight at 105℃±1℃. Calculate the drying loss from the lost weight and the sample weight. 5.6.3 Expression of results
The drying loss X, (expressed as mass percentage) is calculated according to formula (2): Xz= ma=ma× 100
Where: m4 is the mass of the sample, g;
m2 is the mass of the weighing bottle and the sample before drying, g; m3 is the mass of the weighing bottle and the sample after drying, g. 5.7 Specific rotation
5.7.1 Instrument
Polarimeter.
5.7.2 Method
Take 5g of sample (accurate to 0.002g), add water to 50mL, and determine by GB613 method. 5.8 pH
... (2)
5.8.1 Instrument
Acidometer.
5.8.2 Phosphate standard buffer solution (pH6.8) GB16313-1996
Prepare according to page 176 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.8.3 Potassium hydrogen phthalate standard buffer solution (pH4.0) Prepare according to page 39 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.8.4 Method
Take 2g of sample (accurate to 0.01g), add water to 20mL to dissolve. The pH value determination method is used for determination according to the pH value determination method on page 38 of the Appendix of the 1995 edition (Part II) of the Pharmacopoeia of the People's Republic of China.
6 Inspection rules
6.1 This product is inspected by the quality inspection department of the manufacturer according to this standard. The manufacturer guarantees that all products shipped out of the factory meet the requirements of this standard. Each barrel (box) of products shipped out of the factory shall be accompanied by a product inspection certificate. Each batch shall have a product analysis report. 6.2 The product user may conduct quality inspection on the received products according to the inspection rules and test methods specified in this standard to check whether its indicators meet the requirements specified in this standard. 6.3 This product is a batch of finished products with homogeneity after final mixing. 6.4 Sampling Each package is - pieces, each batch is the total number of pieces. When the total number of pieces n≤3, each piece is sampled; when n≤300, the sampling number is Vn→+1: when the total number of pieces n>300, the sampling number is n/2+1; each piece is sampled in equal amounts. After the samples are mixed evenly, the sample is reduced to 8 times the amount of the test by the quartering method, and is divided into two parts and placed in a clean and dry container, labeled. One part is for inspection and analysis, and the other part is sealed and preserved as a reserved sample for arbitration analysis.
6.5 If one indicator does not meet the standard during the inspection, samples should be taken from twice the number of pieces for re-inspection. If one indicator is still unqualified, the batch of products shall be judged as unqualified. 6.6 If the supply and demand parties have objections to the product quality, the statutory arbitration unit may conduct arbitration in accordance with the relevant provisions of this standard. 7 Marking, packaging, transportation and storage
7.1 The packaging should be firmly labeled and marked with the words "food additives", product name, standard number, production license number, registered trademark, net weight, batch number, factory name and address.
7.2 The product is packed in an aluminum-plastic packaging bag that meets the requirements for food and drug packaging, filled with nitrogen, heat-pressed and sealed, placed in a paper barrel (box), and the product certificate is placed. It can also be packaged according to user needs, but the packaging must meet the transportation and storage requirements. 7.3 It must not be mixed with toxic and harmful substances during transportation, and prevent heavy pressure, collision, exposure to the sun and rain. 7.4 This product should be stored in a dark, dry, heat-proof and cool place, and must not be mixed with harmful substances. 7.5 Shelf life The shelf life of the original packaging is one and a half years under the required storage conditions. 2910mL disulfide working solution, shake vigorously for 1min, let stand for stratification, and then perform visual colorimetry. The chromaticity of the trifluoromethane layer of the sample solution shall not be darker than the chromaticity of the trifluoromethane layer of the lead limit standard solution.
5.6 Loss on drying
5.6.1 Instrument
Oven, the sensitivity can be controlled at ±2℃, equipped with a thermometer, the depth of the thermometer inserted into the oven should make the mercury ball and the sample to be tested on the same horizontal plane.
5.6.2 Determination method
Weigh about 3g of the sample, place it in a flat weighing bottle dried to constant weight under the same conditions as the sample, weigh it accurately, dry it to constant weight at 105℃±1℃, and calculate the loss on drying from the lost weight and the sample weight. 5.6.3 Expression of results
The drying loss X, (expressed as mass percentage) is calculated according to formula (2): Xz= ma=ma× 100
Wherein: m4 The mass of the sample, g:
m2——The mass of the weighing bottle and the sample before drying, g; m3
——The mass of the weighing bottle and the sample after drying, g. 5.7 Specific rotation
5.7.1 Instrument
Polarimeter.
5.7.2 Method
Take 5 g of sample (accurate to 0.002 g), add water to 50 mL, and determine by GB613 method. 5.8 pH
... (2)
5.8.1 Instrument
Acidity meter.
5.8.2 Phosphate standard buffer (pH 6.8) GB16313-1996
Prepare according to page 176 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.8.3 Potassium hydrogen phthalate standard buffer (pH 4.0) Prepare according to page 39 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.8.4 Method
Take 2g of sample (accurate to 0.01g), add water to 20mL to dissolve. Determine according to the pH value determination method on page 38 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China.
6 Inspection rules
6.1 This product shall be inspected by the quality inspection department of the manufacturer according to this standard. The manufacturer guarantees that all products shipped out of the factory meet the requirements of this standard. Each barrel (box) of products shipped out of the factory shall be accompanied by a product inspection certificate. Each batch shall have a product analysis report. 6.2 Product users may conduct quality inspections on the products received in accordance with the inspection rules and test methods specified in this standard to check whether their indicators meet the requirements specified in this standard. 6.3 The finished products of this product with homogeneity after final mixing are considered as one batch. 6.4 Sampling Each package is a number of pieces, and each batch is a total number of pieces. When the total number of pieces n≤3, each piece is sampled; when n≤300, the number of samples is Vn→+1: when the total number of pieces n>300, the number of samples is n/2+1; each piece is sampled in equal amounts, and after the samples are mixed evenly, the sample is reduced to 8 times the amount of the test by the quartering method, and divided into two parts and placed in clean and dry containers, labeled, one for inspection and analysis, and the other sealed and stored as a reserved sample for arbitration analysis.
6.5 If one of the indicators does not meet the standard during the inspection, samples should be taken from twice the number of pieces for re-inspection. If one indicator is still unqualified, the batch of products will be judged as unqualified. 6.6 If the supply and demand parties have any objection to the product quality, the statutory arbitration unit may conduct arbitration in accordance with the relevant provisions of this standard. 7 Marking, packaging, transportation and storage
7.1 The packaging should be firmly labeled and marked with the words "food additives", product name, standard number, production license number, registered trademark, net weight, batch number, factory name and address.
7.2 The product is packed in an aluminum-plastic packaging bag that meets the requirements for food and drug packaging, filled with nitrogen, hot-pressed and sealed, placed in a paper barrel (box), and the product certificate is placed. It can also be packaged according to user needs, but the packaging must meet the transportation and storage requirements. 7.3 It must not be mixed with toxic and harmful substances during transportation, and prevent heavy pressure, collision, exposure to the sun, and rain. 7.4 This product should be stored in a dark, dry, heat-proof and cool place, and must not be mixed with harmful substances. 7.5 Shelf life The shelf life of the original packaging is one and a half years under the required storage conditions. 2910mL disulfide working solution, shake vigorously for 1min, let stand for stratification, and then perform visual colorimetry. The chromaticity of the trifluoromethane layer of the sample solution shall not be darker than the chromaticity of the trifluoromethane layer of the lead limit standard solution.
5.6 Loss on drying
5.6.1 Instrument
Oven, the sensitivity can be controlled at ±2℃, equipped with a thermometer, the depth of the thermometer inserted into the oven should make the mercury ball and the sample to be tested on the same horizontal plane.
5.6.2 Determination method
Weigh about 3g of the sample, place it in a flat weighing bottle dried to constant weight under the same conditions as the sample, weigh it accurately, dry it to constant weight at 105℃±1℃, and calculate the loss on drying from the lost weight and the sample weight. 5.6.3 Expression of results
The drying loss X, (expressed as mass percentage) is calculated according to formula (2): Xz= ma=ma× 100
Wherein: m4 The mass of the sample, g:
m2——The mass of the weighing bottle and the sample before drying, g; m3
——The mass of the weighing bottle and the sample after drying, g. 5.7 Specific rotation
5.7.1 Instrument
Polarimeter.
5.7.2 Method
Take 5 g of sample (accurate to 0.002 g), add water to 50 mL, and determine by GB613 method. 5.8 pH
... (2)
5.8.1 Instrument
Acidity meter.
5.8.2 Phosphate standard buffer (pH 6.8) GB16313-1996
Prepare according to page 176 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.8.3 Potassium hydrogen phthalate standard buffer (pH 4.0) Prepare according to page 39 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China. 5.8.4 Method
Take 2g of sample (accurate to 0.01g), add water to 20mL to dissolve. Determine according to the pH value determination method on page 38 of Appendix to the 1995 edition (Volume II) of the Pharmacopoeia of the People's Republic of China.
6 Inspection rules
6.1 This product shall be inspected by the quality inspection department of the manufacturer according to this standard. The manufacturer guarantees that all products shipped out of the factory meet the requirements of this standard. Each barrel (box) of products shipped out of the factory shall be accompanied by a product inspection certificate. Each batch shall have a product analysis report. 6.2 Product users may conduct quality inspections on the products received in accordance with the inspection rules and test methods specified in this standard to check whether their indicators meet the requirements specified in this standard. 6.3 The finished products of this product with homogeneity after final mixing are considered as one batch. 6.4 Sampling Each package is a number of pieces, and each batch is a total number of pieces. When the total number of pieces n≤3, each piece is sampled; when n≤300, the number of samples is Vn→+1: when the total number of pieces n>300, the number of samples is n/2+1; each piece is sampled in equal amounts, and after the samples are mixed evenly, the sample is reduced to 8 times the amount of the test by the quartering method, and divided into two parts and placed in clean and dry containers, labeled, one for inspection and analysis, and the other sealed and stored as a reserved sample for arbitration analysis.
6.5 If one of the indicators does not meet the standard during the inspection, samples should be taken from twice the number of pieces for re-inspection. If one indicator is still unqualified, the batch of products will be judged as unqualified. 6.6 If the supply and demand parties have any objection to the product quality, the statutory arbitration unit may conduct arbitration in accordance with the relevant provisions of this standard. 7 Marking, packaging, transportation and storage
7.1 The packaging should be firmly labeled and marked with the words "food additives", product name, standard number, production license number, registered trademark, net weight, batch number, factory name and address.
7.2 The product is packed in an aluminum-plastic packaging bag that meets the requirements for food and drug packaging, filled with nitrogen, hot-pressed and sealed, placed in a paper barrel (box), and the product certificate is placed. It can also be packaged according to user needs, but the packaging must meet the transportation and storage requirements. 7.3 It must not be mixed with toxic and harmful substances during transportation, and prevent heavy pressure, collision, exposure to the sun, and rain. 7.4 This product should be stored in a dark, dry, heat-proof and cool place, and must not be mixed with harmful substances. 7.5 Shelf life The shelf life of the original packaging is one and a half years under the required storage conditions. 291
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