Some standard content:
National Standard of the People's Republic of China
Food additive
Calcium ascorbate
1 Subject content and applicable scope
GB15809—1995
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage requirements of food additive calcium ascorbate.
This standard applies to calcium ascorbate made from ascorbic acid and calcium salts, which is used as an antioxidant and nutritional enhancer in the food industry.
2 Reference standards
GB601 Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents GB613 General method for determination of specific rotation of chemical reagents GB5009.18 Determination of fluorine in foods
GB8450 Determination of arsenic in food additives Pharmacopoeia of the People's Republic of China, 1990 edition (Part II) 3 Chemical name, molecular formula, structural formula, molecular weight Chemical name: Calcium ascorbate
English name: Calcium ascorbate
Molecular formula: C12H,CaO12·2H,O
Structural formula:
Ca2+·2H,0
Molecular weight: 426.35 (according to the international atomic weight of 1987) 4 Technical requirements
4.1 Properties
This product is a white or light yellow crystalline powder, odorless, soluble in water, slightly soluble in ethanol, insoluble in ether. 4.2 Items and indicators
Approved by the State Bureau of Technical Supervision on December 8, 1995, and implemented on August 1, 1996
Content (calculated as Ci2H1aCa()12·2H2O), %Specific rotation [α
Monument (calculated as As), %
Fluoride, %
Heavy metal (calculated as Pb), %
Oxalate test
PH (10% aqueous solution)
Test method
GB15809--1995www.bzxz.net
+95°～+97°
6. 8~7. 4
The reagents used in this standard are analytically pure reagents. Water is distilled water or water of corresponding purity. Solutions not specified are aqueous solutions. 5.1 Identification
5.1.1 Reagents and solutions
Methyl red test solution: Take 0.1g of methyl red and add 7.4ml of 0.05mol/L sodium hydroxide (GB629) solution to dissolve it. Then add water to dilute to 200ml. Color change range: pH 4.2～6.3 (test solution changes from red to yellow); b.
Ammonia test solution: take 400mL of ammonia water (GB831), add water to dilute to 1000mL, and obtain; dilute hydrochloric acid: take 234mL of hydrochloric acid (GB622), add water to dilute to 1000mL, and obtain; ammonium oxalate test solution: take 3.5g of ammonium oxalate (HG3--976), add water to dissolve to 100mL, and obtain; d.
Sodium dichloroindophenolate test solution: take 0.1g of sodium 2,6-dichloroindophenolate, add water to dissolve it, and filter it to obtain. 5.1.2 Identification method
5.1.2.1 Take 1g sample and dissolve it in 10mL water, add 2 drops of methyl red indicator solution, neutralize with nitrogen test solution, and then add hydrochloric acid until it is just acidic; add ammonium oxalate test solution, and a white precipitate will be generated; separate, the precipitate is insoluble in acetic acid, but soluble in hydrochloric acid, 5.1.2.2 Take 1g sample and dissolve it in 10mL water, add 2 drops of sodium dichloroindophenol test solution, and the sodium dichloroindophenol test solution will fade. 5.2 Determination of calcium ascorbate content
5.2.1 Principle
The ascorbic acid in this product can be quantitatively oxidized to dehydroascorbic acid by iodine, and the titration end point is determined by the color of the iodine titrant. 0
5.2.2 Reagents and solutions
Iodine (GB675);
Ca2t+212
2HOCH2
0+ Calz + 2HI
b, iodine standard titration solution: 0.1mol/L iodine standard titration solution is prepared and calibrated according to GB601 method. 5.2.3 Determination method
Weigh about 0.3g of sample, put it in a 25)ml conical flask, add 50mL of water to dissolve it, and immediately titrate it with iodine standard titration solution (0.1mol/L) until the solution turns light yellow and does not fade within 30s. Each 1mL of iodine solution (0.1mol/L) is equivalent to 0.01066g of C2HiCa0Oz·2H,O.
5.2.3.1 Expression of analysis results
The content of calcium ascorbate is calculated according to the following formula:
GB15809--1995
X= Y·FX 0. 010 66 × 100
Wherein: V-the volume of standard iodine titration solution consumed by the sample, mL; F——the conversion value of the concentration of standard iodine titration solution: F=the measured concentration of the titration wave (mol/L); the mass of the sample, g;
the specified concentration of the titration solution (mol/L);
0.01066-the mass of calcium ascorbate (C,HCaO: 2H,O) in grams equivalent to 1.00mL of standard iodine titration solution [c (1/21z) = 0.1 mol/L].
5.2.4 Allowable difference
The relative deviation of the results of two parallel determinations of this method shall not exceed 0.3%. 5.3 Specific rotation
5.3.1 Instrument
Polarimeter.
5.3.2 Method
Take 1g of sample and add water to 25mL, and determine according to GB613. 5.4 Determination of arsenic salts
5.4.1 Reagents and solutions
Hydrochloric acid (GB622);
Arsenic standard solution: prepared according to GB8450. 1.0mL of this solution is equivalent to 1.0μg of stele. 5.4.2 Determination method
Take 3g of sample and determine by the GB8450 arsenic spot method. 5.5 Determination of fluoride
5.5.1 Reagents and solutions
Sodium fluoride (GB1264);
b. Fluoride standard solution: Prepared according to GB5009.18, 1.0 mL of this solution is equivalent to 5 μg of fluoride. 5.5.2 Determination method
Weigh 5 g of sample and determine according to the ashing distillation-fluorine reagent colorimetric method in GB5009.18. 5.6 Determination of heavy metals
5.6.1 Reagents and solutions
6mol/L hydrochloric acid: take 50mL hydrochloric acid (GB622) and dilute it to 100mL with water. 1% nitric acid: take 1ml. nitric acid (GB627) and dilute it to 100mL with water. b.
pH3.5 acetate buffer: weigh 25.0g ammonium acetate (GB1292) and dissolve it in 25mL water, add 45mL.6mol/L hydrochloric acid c
adjust the pH value to 3.5 with dilute hydrochloric acid or dilute ammonia water, dilute it to 100mL with water. d. Thioacetamide solution: weigh 4g thioacetamide, add water to dissolve it into 100mL, and store it in a refrigerator. Before use, take 5.0 mL of the mixed solution [15 mL of sodium hydroxide solution (1 mol/L), 5.0 mL of water and 20 mL of glycerol, mix and shake well], add 1.0 mL of this solution, heat in a water bath for 20 seconds, cool, and use immediately; e Lead standard solution: weigh 0.1598 g of high-purity lead nitrate (HG3--1309), dissolve it in 10 mL of 1% nitric acid, quantitatively transfer it into a 100 mL volumetric flask, and dilute it to the mark with water. 1 mL of this solution is equivalent to 1.0 mg of lead. Dilute it 100 times with water before use, so that 1.0 mlL is equivalent to 10 μg of lead.
5.6.2 Determination method
5.6.2.7A tube: Take a 50 mL Nessler colorimetric tube, add 2.0 mL of lead standard solution and 2 mL of pH 3.5 acetate buffer to the tube, and dilute it to 25 mL with water.
5.6.2.2 Tube B: Take the 50mL Nessler colorimetric tube that matches tube A, add 2g of sample to the tube, and add water to 25ml. 5.6.2.3 Add 2ml of thioacetamide solution to tubes A and B respectively, and add water to 50ml, mix well, and let stand for 2min. Observe under a white background. The color of tube B shall not be darker than that of tube A. 5.7 Oxalate test
5.7.1 Reagents and solutions
a. Glacial acetic acid (GB 676);
b Calcium acetate (HGB3126); 10% solution.
5.7.2 Determination method
Take 1g of sample, add 10ml of water, add 2 drops of glacial acetic acid and 5mL of 10% calcium acetate solution, and let stand for 5min. The solution should remain clear. 5.8 Determination of acidity
Take 5g of sample and add water to 50mL, and determine the pH value. 6 Inspection rules
6.1 This product shall be inspected by the quality inspection department of the manufacturer in accordance with this standard. The manufacturer guarantees that all products shipped out of the factory meet the requirements of this standard. Each barrel of products shipped out of the factory shall be accompanied by a product inspection certificate. 6.2 The user may conduct quality inspection on the received products in accordance with the inspection rules and test methods specified in this standard to check whether their indicators meet the requirements of this standard.
6.3 This product is a batch of finished products with uniformity after final mixing. 6.4 Sampling method and sampling quantity
Each package is one piece. When the total number of pieces n≤3, each piece is sampled. When n≤300, the sampling number is √n+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 and evenly hooked, use the quartering method to reduce the sample to 8 times the amount of the test, and put it into two clean containers, label it, one for inspection and analysis, and the other 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 Packaging, marking, 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 available in two specifications of 5kg and 25kg. The product is packed in two layers of polyethylene bags, nitrogen-filled and heat-pressed, and then covered with a kraft paper bag and sealed in a cardboard drum or carton. 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 hazardous substances during transportation to prevent heavy pressure, Collision, exposure to sunlight, and rain. 7.4 This product should be stored in a dark, dry, heat-proof and cool place, and should not be mixed with harmful substances. 7.5 Shelf life: The shelf life is one and a half years in the original packaging under the required storage conditions. Additional instructions:
This standard is proposed by the State Food and Drug Administration. This standard is technically managed by China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. This standard was drafted by Hubei Yichang Pharmaceutical Factory. The main drafters of this standard are Yuan Ermin, Cai Tao, and Fang Qun. This standard is equivalent to the 1983 direct version of the US Food and Chemicals Regulations (FCC). 288
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