Some standard content:
GB17203-·1998
This standard is equivalent to the provisions of the United States Pharmacopoeia (UPS) 23rd edition of calcium citrate. Among them, the indicators of loss on drying, fluoride, hydrochloric acid insoluble matter, heavy metals and stelae are all in accordance with the provisions of USP23 edition, and the content and lead indicators are better than those of USP23 edition. The inspection methods of this standard adopt USP23 edition and Part II of the 1995 edition of the Pharmacopoeia of the People's Republic of China and relevant national standards. This standard was proposed by the Food and Papermaking Department of the China Light Industry Association. This standard is technically managed by the National Food Fermentation Standardization Center and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai Dadong Calcium Citrate Factory and China Food Fermentation Industry Research Institute. The main drafters of this standard are Yuan Qun and Wu Yuhong. 300
1 Scope
National Standard of the People's Republic of China
Food additive
Calcium citrate
Food additive
Calcium citrate
GB 17203 -- 1998
This standard specifies the technical requirements, test methods, inspection rules and various requirements for packaging, labeling, storage and transportation of food additive calcium citrate.
This standard applies to calcium citrate synthesized from citric acid and calcium carbonate, which is used as a nutritional enhancer in the food industry. 2 Referenced 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. GB8449--87 Determination of lead in food additives GB8451--87 Test method for heavy metal limits in food additives Appendix 3 to Part II of the 1995 edition of the Pharmacopoeia of the People's Republic of China Structural formula, molecular weight
Structural formula:
CH,CO0O-
Molecular formula: C12HioCa:O·4H20
CH,COO-
Molecular weight: 570.50 (according to the 1993 international atomic weight) Chemical name: 2-hydroxypropane-1,2,3-tricarboxylic acid calcium tetrahydrate 4 Technical requirements
4.1 Appearance: white crystalline powder.
4.2 Physical and chemical indicators are shown in Table 1.
Approved by the State Technical Supervision Bureau on January 16, 1998Ca2+ 4H20
Implementation on December 1, 1998
Content [as Cas(C,HsO,)], %
Loss on drying, %
Hydrochloric acid insoluble matter, %
Lead (Pb), %
Heavy metal (as Pb), %
Arsenic (As), %
Fluoride (as F), %
Clarity of solutionWww.bzxZ.net
5 Test method
GB17203-—1998
98.0100.5
The reagents and water used in this standard, unless otherwise specified, shall be of analytical grade reagents and distilled water or water of equivalent purity. 5.1 Identification
5.1.1 Reagents and solutions
5.1.1.1 Hydrochloric acid (GB622).
5.1.1.2 1mol/L acetic acid (GB676) solution. 5.1.1.3 1mol/L mercuric sulfate solution.
5.1.1.4 1mol/L potassium permanganate (GB643) solution. 5.1.1.5 1mol/L ammonium oxalate (HG3-976) solution. 5.1.1.6 2mol/L nitric acid (GB626) solution: 125mL concentrated nitric acid is diluted to 1000mL with water. 5.1.2 Identification test
Method 1: Dissolve 0.5g sample in a mixture of 10mL water and 2.5mL 2mol/L nitric acid, add 1mL 1mol/L mercuric sulfate solution, heat to boiling, and then add 1ml 1mal/L potassium permanganate solution to produce a white precipitate. Method 2: Completely burn 0.5g sample at the lowest possible temperature, then cool, and dissolve the residue in a mixture of 10mL water and 1mL 1mol/L acetic acid. After filtering, add 10mL 1mol/L ammonium oxalate solution to the filtrate to produce a large volume of white precipitate that can be dissolved in hydrochloric acid.
5.2 Determination of content
5.2.1 Reagents and solutions
5.2.1.1 3mol/L hydrochloric acid solution.
5.2.1.2 6mol/L hydrochloric acid solution.
5.2.1.31mol/L sodium hydroxide (GB629) solution: accurately weigh 4g sodium hydroxide, dissolve in water, and dilute to 100mL. 5.2.1.430% triethanolamine solution: dilute 38mL triethanolamine with water to 100mL. 5.2.1.5 Calcium indicator: weigh 10g sodium chloride that has been dried at 105-110℃ for 2h, grind it in a mortar, add 0.1g calcium reagent, grind it, and mix it.
5.2.1.60.05mol/L disodium ethylenediaminetetraacetate (EDTA-2Na) standard solution preparation: weigh 20g disodium ethylenediaminetetraacetate (GB1401), heat it and dissolve it in 1000mL water, cool it, and shake it well. Calibration: weigh 1g standard zinc oxide burned to constant weight at 800℃, and weigh it to 0.0002g. Moisten with a little water, add 6mol/L hydrochloric acid until the sample dissolves, transfer to a 250mL volumetric flask, dilute to scale, and shake well. Take 30.00~~35.00mL, add 70ml water, neutralize to pH7~~8 with 10% nitrogen water, add 10mL ammonia-ammonium chloride buffer solution A (pH10), add 5 drops of 0.5% chrome black T indicator solution, and titrate with 0.05mol/L disodium ethylenediaminetetraacetic acid solution until the solution changes from purple to pure blue. Perform a blank test at the same time. 302
Calculation:
In the formula: c
GB 17203—1998
m×250
c= (V,-V,)X0. 08138
Concentration of disodium ethylenediaminetetraacetic acid standard solution; Volume of zinc oxide solution consumed, mL;
Mass of zinc oxide, g,
Volume of disodium ethylenediaminetetraacetic acid solution consumed, mL; Vz
V3\—Volume of disodium ethylenediaminetetraacetic acid solution consumed in the blank test, mL; 0.08138—Number of grams of zinc oxide per milliliter of 1 mol/l. 5.2.2 Determination method
Pre-dry at 150℃ to constant weight, accurately weigh 350-400mg calcium citrate sample (weighing to 0.0001g), add 10mL of water and 3mol/L hydrochloric acid until dissolved (about 2mL), dilute with water to about 100mL, add 5mL of 30% triethanolamine and 15mL of 1mol/L sodium hydroxide, shake to hook. Adjust the pH value to greater than 13, add about 0.1g of calcium indicator, and titrate with 0.05mol/L disodium ethylenediaminetetraacetic acid standard solution until the solution changes from purple-red to pure blue as the end point. 5.2.3 Expression of analysis results
Calcium citrate content [X (%)] is calculated according to formula (2): X (%) = VX8.307XF
m×1 000
Wherein: V--the volume of 0.05mol/L disodium ethylenediaminetetraacetic acid standard solution consumed, mL; F--the ratio of the actual concentration of 0.05mol/L disodium ethylenediaminetetraacetic acid standard solution to 0.05; m
The mass of the sample, g;
8.307--Each 1ml.0.05mol/L ethylenediaminetetraacetic acid salt consumed is equivalent to 8.307mg of calcium citrate. 5.3 Determination of loss on drying
Weigh 2g of the sample (accurate to 0.0001g), dry it at 150℃ for 4h, and determine it according to the Appendix of Part II of the 1995 edition of the Pharmacopoeia of the People's Republic of China.
5.4 Determination of hydrochloric acid insoluble matter
Weigh 5g of sample (accurate to 0.001g), add 10mL of 6mol/L hydrochloric acid (5.2.1.2) and 50mL of water, mix and heat for 30min, filter the resulting solution with a clean No. 3 quartz sand core funnel that has been dried at 105℃ for 2h and cooled and weighed, and then filter and wash with 200mL of water for 5 times, dry the precipitate in an oven at 105℃ for 2h, cool and weigh, and the residue should not weigh more than 10mg (i.e. 0.2%). 5. 5 Determination of arsenic
Dissolve 1g of sample (accurate to 0.001g), add 5mL of 3mol/L hydrochloric acid (5.2.1.1) to dissolve, dilute to 35mL with water, use this solution as the test solution, and determine according to the second method on page 56 of the Appendix to Part II of the 1995 edition of the Chinese Pharmacopoeia. 5.6 Determination of heavy metals
Determination shall be carried out in accordance with GB8451.
5.7 Determination of lead
Determine according to the method of GB8449.
5.8 Determination of fluoride
5.8.1 Reagents and solutions
5.8.1.1 Perchloric acid (GB623).
5.8.1.2 Nitric acid solution: weigh 250mg of nitric acid solution, dissolve it in water and dilute it to 1000mL. 5.8.1.3 Alizarin sodium sulfonate solution (1-1000). 0.05mol/L sodium hydroxide (GB629) solution. 5.8. 1.4
5.8. 1.5 0. 1Lmol/L hydrochloric acid (GB 622). GB 17203-1998
5.8.1.6 Sodium fluoride standard solution: Accurately weigh 22.1 mg of sodium fluoride (GB1264) dried at 105°C for 1 hour, place in a 100 mL volumetric flask, add water to dissolve and dilute to the mark, shake well; accurately measure 10 mL, place in another 100 ml volumetric flask, add water to dilute to the mark, shake well, and you will get 10 g of fluorine per 1 mL of sodium fluoride standard solution. 5.8.2 Instruments and equipment
General laboratory instruments and
5.8.2.1 Fluorine measurement device by distillation (see Figure 1). 5.8.2.2 Colorimetric tube 50 ml.
1--Steam generator (1000mL flask); 2-Safety tube ($5mm); 3---Glass tube ($5mm); 4-Rubber stopper; 5-Tee pipe and screw clamp: 6-Thermometer (200℃): 7-Three-necked flask (250mL); 8-Glass elbow; 9 Straight condenser (500mm); 10Glass elbow; 11-Volume flask; 12-Heating jacket or electric furnace; 13, 14-Rubber stopper Figure 1 Schematic diagram of fluorine measurement
5.8.3 Operation method
Weigh 2.0g of sample (accurate to 0.1g), put it in a 250mL three-necked flask (see Figure 1), add 10 to 20 glass beads, slowly add 5ml of perfluoric acid, and rinse the flask wall with 15ml of water. Install a thermometer and a glass tube on the three-necked flask, and insert the mercury ball and the glass tube of the thermometer into the test solution in the three-necked flask, and connect the three-necked flask with the steam generator and the straight condenser according to the fluorine measurement schematic diagram, add 500mL of water into the steam generator, open the screw clamp, heat to boiling, close the screw clamp, pass water vapor into the three-necked flask, and use an electric furnace to keep the liquid in the three-necked flask at 135-140℃ until the distillate is about 70ml. Stop distillation. Dilute the distillate to 80mL with water, mix, transfer 40ml of the solution to a 50ml colorimetric tube, and fill the same tube with 40ml as a control tube. Add 0.1ml of sodium alizarin sulfonate solution to half of the tube containing the distillate until the sample tube turns pink (1-1000), mix, drop 0.05mol/L sodium hydroxide solution, stir until it is consistent with the control arm, then add 1ml of 0.1mol/L hydrochloric acid to each sample and control tube, mix. Add nitric acid solution to the sample tube with a burette in an amount of 0.05ml each time to make the sample solution turn pink. At the same time, add the same volume of nitric acid solution to the control tube, mix, and then use a burette to add sodium fluoride standard solution. After the sample tube and the control tube have the same color, dilute to the same volume, mix, and let the bubbles in the tube escape. After comparison, add 1 to 2 drops of sodium fluoride standard solution to the control tube. If the color of the solution changes significantly (i.e., the color of the solution in the control tube is significantly darker than that of the sample tube), the end point can be determined. The consumption of sodium fluoride standard solution shall not exceed 3.0 mL (0.003%). Each 1 ml of sodium fluoride standard solution is equivalent to 10 g of fluoride. 5.9 Determination of solution clarity Weigh 5 g of the sample, mix and heat with 5 ml of 37% hydrochloric acid and 50 ml of water, and then dilute to 100 ml with water. Determine according to Appendix IXB "Clarity Test Method" of Part II of the 1995 edition of the Pharmacopoeia of the People's Republic of China GB 17203-1998. 6 Inspection rules
6.1 This product should be inspected and qualified by the factory quality inspection department according to the requirements of this standard, and can only be packaged and put into the warehouse or shipped out of the factory after the certificate of conformity is attached. 6.2 The products produced by each batch are considered as one batch. 6.3 Take samples according to 5% of the total number of product packaging units, and evenly sample 200g from each packaging unit, with a total amount of not less than 400g. Mix the obtained samples evenly, and use the quartering method to reduce them to about 100g, and put them into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number, quantity and sampling date. One bottle is for testing, and the other bottle is kept for reference. 6.4 Content, drying loss and hydrochloric acid insoluble matter are mandatory inspection items, and other indicators are type inspection items, which are inspected once every six months. If one of the indicators in the inspection does not meet the requirements of this standard, re-sampling can be carried out from the packaged products, with the number of sampling barrels not less than 10 barrels and the total mass of the samples being about 400g. After mixing and evenly rubbing, all items shall be re-inspected. If one of the inspection results is still unqualified, the batch of products shall be judged as unqualified. 6.5 The user unit may inspect the quality of the received products according to the technical requirements, inspection rules and test methods specified in this standard to check whether its indicators meet the requirements of this standard. 6.6 When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution shall be selected by both parties through consultation. During arbitration, arbitration analysis shall be carried out in accordance with the inspection methods specified in this standard.
7 Packaging, marking, storage and transportation
7.1 Packaging
The products are packed in food-grade polyethylene film bags, which are sealed by heat and pressure. The average mass of each hundred bags is not less than 25kg, and cardboard barrels are used as outer packaging.
7.2 Marking
The product packaging should be firmly marked with the manufacturer's name, factory address, product name, trademark, product model, batch number, production date, shelf life, main parameters of the product, net content and product standard number, and marked with the words "food additives". 7.3 Storage
The product should be stored in a dry, ventilated and clean place, and avoid being piled up with toxic, harmful, perishable and easily contaminated items. 7.4 Transportation
The product must be loaded and unloaded gently during transportation, and must not be mixed with harmful, toxic and easily contaminated items. It must be strictly protected from rain and exposure. 8 Shelf Life
The shelf life is one year if the specified storage and transportation conditions are met and the packaging is intact and the seal is not opened. 305Stop distillation. Dilute the distillate to 80mL with water, mix, transfer 40ml of the solution to a 50ml colorimetric tube, and fill the same tube with 40ml as a control tube. Add 0.1ml of sodium alizarin sulfonate solution to half of the tube containing the distillate until the sample tube turns pink (1-1000), mix, drop 0.05mol/L sodium hydroxide solution, stir until it is consistent with the control arm, then add 1ml of 0.1mol/L hydrochloric acid to each of the sample and control tubes, mix. Add nitric acid solution to the sample tube with a burette in an amount of 0.05ml each time to make the sample solution turn pink. At the same time, add the same volume of nitric acid solution to the control tube, mix, and then use a burette to add sodium fluoride standard solution. After the sample tube and the control tube have the same color, dilute to the same volume, mix, and let the bubbles in the tube escape. After comparison, add 1 to 2 drops of sodium fluoride standard solution to the control tube. If the color of the solution changes significantly (i.e., the color of the solution in the control tube is significantly darker than that of the sample tube), the end point can be determined. The consumption of sodium fluoride standard solution shall not exceed 3.0 mL (0.003%). Each 1 ml of sodium fluoride standard solution is equivalent to 10 g of fluoride. 5.9 Determination of solution clarity Weigh 5 g of the sample, mix and heat with 5 ml of 37% hydrochloric acid and 50 ml of water, and then dilute to 100 ml with water. Determine according to Appendix IXB "Clarity Test Method" of Part II of the 1995 edition of the Pharmacopoeia of the People's Republic of China GB 17203-1998. 6 Inspection rules
6.1 This product should be inspected and qualified by the factory quality inspection department according to the requirements of this standard, and can only be packaged and put into the warehouse or shipped out of the factory after the certificate of conformity is attached. 6.2 The products produced by each batch are considered as one batch. 6.3 Take samples according to 5% of the total number of product packaging units, and evenly sample 200g from each packaging unit, with a total amount of not less than 400g. Mix the obtained samples evenly, and use the quartering method to reduce them to about 100g, and put them into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number, quantity and sampling date. One bottle is for testing, and the other bottle is kept for reference. 6.4 Content, drying loss and hydrochloric acid insoluble matter are mandatory inspection items, and other indicators are type inspection items, which are inspected once every six months. If one of the indicators in the inspection does not meet the requirements of this standard, re-sampling can be carried out from the packaged products, with the number of sampling barrels not less than 10 barrels and the total mass of the samples being about 400g. After mixing and evenly rubbing, all items shall be re-inspected. If one of the inspection results is still unqualified, the batch of products shall be judged as unqualified. 6.5 The user unit may inspect the quality of the received products according to the technical requirements, inspection rules and test methods specified in this standard to check whether its indicators meet the requirements of this standard. 6.6 When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution shall be selected by both parties through consultation. During arbitration, arbitration analysis shall be carried out in accordance with the inspection methods specified in this standard.
7 Packaging, marking, storage and transportation
7.1 Packaging
The products are packed in food-grade polyethylene film bags, which are sealed by heat and pressure. The average mass of each hundred bags is not less than 25kg, and cardboard barrels are used as outer packaging.
7.2 Marking
The product packaging should be firmly marked with the manufacturer's name, factory address, product name, trademark, product model, batch number, production date, shelf life, main parameters of the product, net content and product standard number, and marked with the words "food additives". 7.3 Storage
The product should be stored in a dry, ventilated and clean place, and avoid being piled up with toxic, harmful, perishable and easily contaminated items. 7.4 Transportation
The product must be loaded and unloaded gently during transportation, and must not be mixed with harmful, toxic and easily contaminated items. It must be strictly protected from rain and exposure. 8 Shelf Life
The shelf life is one year if the specified storage and transportation conditions are met and the packaging is intact and the seal is not opened. 305Stop distillation. Dilute the distillate to 80mL with water, mix, transfer 40ml of the solution to a 50ml colorimetric tube, and fill the same tube with 40ml as a control tube. Add 0.1ml of sodium alizarin sulfonate solution to half of the tube containing the distillate until the sample tube turns pink (1-1000), mix, drop 0.05mol/L sodium hydroxide solution, stir until it is consistent with the control arm, then add 1ml of 0.1mol/L hydrochloric acid to each of the sample and control tubes, mix. Add nitric acid solution to the sample tube with a burette in an amount of 0.05ml each time to make the sample solution turn pink. At the same time, add the same volume of nitric acid solution to the control tube, mix, and then use a burette to add sodium fluoride standard solution. After the sample tube and the control tube have the same color, dilute to the same volume, mix, and let the bubbles in the tube escape. After comparison, add 1 to 2 drops of sodium fluoride standard solution to the control tube. If the color of the solution changes significantly (i.e., the color of the solution in the control tube is significantly darker than that of the sample tube), the end point can be determined. The consumption of sodium fluoride standard solution shall not exceed 3.0 mL (0.003%). Each 1 ml of sodium fluoride standard solution is equivalent to 10 g of fluoride. 5.9 Determination of solution clarity Weigh 5 g of the sample, mix and heat with 5 ml of 37% hydrochloric acid and 50 ml of water, and then dilute to 100 ml with water. Determine according to Appendix IXB "Clarity Test Method" of Part II of the 1995 edition of the Pharmacopoeia of the People's Republic of China GB 17203-1998. 6 Inspection rules
6.1 This product should be inspected and qualified by the factory quality inspection department according to the requirements of this standard, and can only be packaged and put into the warehouse or shipped out of the factory after the certificate of conformity is attached. 6.2 The products produced by each batch are considered as one batch. 6.3 Take samples according to 5% of the total number of product packaging units, and evenly sample 200g from each packaging unit, with a total amount of not less than 400g. Mix the obtained samples evenly, and use the quartering method to reduce them to about 100g, and put them into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number, quantity and sampling date. One bottle is for testing, and the other bottle is kept for reference. 6.4 Content, drying loss and hydrochloric acid insoluble matter are mandatory inspection items, and other indicators are type inspection items, which are inspected once every six months. If one of the indicators in the inspection does not meet the requirements of this standard, re-sampling can be carried out from the packaged products, with the number of sampling barrels not less than 10 barrels and the total mass of the samples being about 400g. After mixing and evenly rubbing, all items shall be re-inspected. If one of the inspection results is still unqualified, the batch of products shall be judged as unqualified. 6.5 The user unit may inspect the quality of the received products according to the technical requirements, inspection rules and test methods specified in this standard to check whether its indicators meet the requirements of this standard. 6.6 When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution shall be selected by both parties through consultation. During arbitration, arbitration analysis shall be carried out in accordance with the inspection methods specified in this standard.
7 Packaging, marking, storage and transportation
7.1 Packaging
The products are packed in food-grade polyethylene film bags, which are sealed by heat and pressure. The average mass of each hundred bags is not less than 25kg, and cardboard barrels are used as outer packaging.
7.2 Marking
The product packaging should be firmly marked with the manufacturer's name, factory address, product name, trademark, product model, batch number, production date, shelf life, main parameters of the product, net content and product standard number, and marked with the words "food additives". 7.3 Storage
The product should be stored in a dry, ventilated and clean place, and avoid being piled up with toxic, harmful, perishable and easily contaminated items. 7.4 Transportation
The product must be loaded and unloaded gently during transportation, and must not be mixed with harmful, toxic and easily contaminated items. It must be strictly protected from rain and exposure. 8 Shelf Life
The shelf life is one year if the specified storage and transportation conditions are met and the packaging is intact and the seal is not opened. 305
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