Some standard content:
National Standard of the People's Republic of China
Food additive
Calcium gluconate
Food additive-Calcium gluconate1Subject content and scope of application
GB15571-1995
This standard specifies the technical requirements, inspection methods, inspection rules, marking packaging, transportation and storage requirements for food additive calcium gluconate.
This standard applies to calcium gluconate produced by fermentation with starch as raw material, which is used as a nutritional enhancer in the food industry. 2 Reference standards
GB8450 Determination of calcium in food additives GB8451 Test method for heavy metal limits in food additives Part II of the 1990 edition of the Pharmacopoeia of the People's Republic of China 3 Chemical name, molecular formula, structural formula, molecular weight Chemical name: Calcium gluconate
Molecular formula: C12H22CaO14·H20
Structural formula;
HOH,C-
Molecular weight: 448.39
4 Technical requirements
4.1 Properties
Ca2+H,O
This product is white crystalline powder or granular powder, odorless and tasteless. It is easily soluble in boiling water and slowly dissolved in water. It is insoluble in anhydrous ethanol, trifluoromethane or ether. 4.2 Items and indicators
Approved by the State Bureau of Technical Supervision on June 2, 1995, and implemented on December 1, 1995
Content (in C12H2CaOi·HO), %
Arsenic salt (in As), %
Heavy metal (in Pb), %
Loss on drying, %
Sucrose or reducing sugar
Chloride, %
Sulfate, %
5 Test method
GB155711995
99.0~102. 0
Red precipitate shall not be produced immediately
The reagents used in the test of this standard are analytically pure reagents, water is distilled water or water of corresponding purity, and solutions not specified are aqueous solutions. 5.1 Identification
5.1.1 Reagents and solutions
5.1.1.1 Glacial acetic acid (GB1628).
5.1.1.2 Benzene: freshly distilled reagent.
5.1.1.3 Ferric chloride solution: Take 9g of ferric chloride and add water to dissolve it into 100mL. 5.1.2 Identification method
5.1.2.1 Take 1g of this product and add 40mL of water to dissolve it. Take this solution and test it according to page 39 of Appendix II of the 1990 edition of the Pharmacopoeia of the People's Republic of China. The identification reaction of calcium salt should be shown. 5.1.2.2 Take 0.5g of this product, put it in a test tube, add 5mL of water, dissolve it with slight heat, add 0.7mL of glacial acetic acid and 1mL of freshly distilled benzene, heat it in a water bath for 30 minutes, then let it cool to room temperature. Rub the inner wall of the test tube with a glass rod, and yellow crystals will gradually form. 5.1.2.3 Take about 0.1g of this product, add 5mL of water to dissolve, add 1 drop of ferric chloride test solution, and it will turn dark yellow. 5.2 Determination of calcium gluconate content
5.2.1 Reagents and solutions
5.2.1.1 Sodium hydroxide (GB629): c=1mol/L solution. 5.2.1.2 Disodium ethylenediaminetetraacetic acid (GB1401) standard titration solution: c=0.05mol/L. 5.2.1.3 Calcium purpurogenous pigment indicator: Take 0.1g of calcium purpurogenous pigment, add 10g of anhydrous sodium sulfate, and grind evenly. 5.2.2 Determination method
Take 0.5g of this product, weigh accurately (accurate to 0.0001g), add 100mL of water, heat slightly to dissolve, bring to room temperature, add 15mL of sodium hydroxide solution and 0.1g of calcopurpurin indicator, and titrate with 0.05mol/L disodium ethylenediaminetetraacetic acid standard titration solution until the solution changes from purple to pure blue.
5.2.3 Expression of analysis results
Calcium gluconate content (X1) is expressed as mass percentage and is calculated according to formula (1): V:c X 0. 448 4
Wherein: V
Volume of disodium ethylenediaminetetraacetic acid standard titration solution, ml; Actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L; (1)
Mass of sample, gram;
GB15571--1995
0.4484--Mass of calcium gluconate equivalent to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution [c(EDTA)=1.000mol/L] in grams.
The result is taken as the arithmetic mean of two parallel determinations, and two decimal places are retained. 5.2.4 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed 0.3%. 5.3 Determination of arsenic saltsbzxZ.net
5.3.1 Reagents and solutions
5.3.7.1 Hydrochloric acid (GB622) reagent.
5.3.1.2 Standard arsenic stock solution: Weigh 0.132g of arsenic trioxide, place it in a 1000mL volumetric flask, add 5mL of 20% sodium hydroxide solution to dissolve, neutralize with an appropriate amount of dilute sulfuric acid, add 10mL of dilute sulfuric acid, dilute to the scale with water, and spread evenly. 5.3.1.3 Standard arsenic solution: Before use, accurately measure 10mL of standard arsenic stock solution, place it in a 1000mL volumetric flask, add 10mL of dilute sulfuric acid, dilute to the scale with water, and shake evenly.
5.3.2 Determination method
5.3.2.1 Method 1
Take 1g of this product and determine it according to the arsenic spot method in GB8450. 5.3.2.2 Method 2
Take 1g of this product, add 5mL of hydrochloric acid reagent, dissolve it with 23mL of water, and determine it according to the Gu Cai method on page 53 of Appendix II of the 199th edition of the Pharmacopoeia of the People's Republic of China.
5.4 Determination of heavy metals
5.4.1 Reagents and solutions
5.4.1. 1 Hydrochloric acid (GB622) solution: 1 mol/1. 5.4.1.2 Acetate buffer (pH 3.5): Take 25g of ammonium acetate, add 25mL of water to dissolve, add 38mL of hydrochloric acid solution (7mol/L), use hydrochloric acid solution (2mol/L) or ammonia solution (5mol/L) to accurately adjust the pH to 3.5 (indicated by potentiometric method), dilute with water to 100mL, and shake well. 5.4.1.3 Thioacetamide solution: Take 4g of thioacetamide, add water to dissolve to 100mL, and store in a refrigerator. Before use, take 5.0mL of the mixed solution (5.4.1.4), add 1.0mL of this solution, heat in a water bath for 20s, cool, and use immediately. 5.4.1.4 Mixed solution: Take 15mL of sodium hydroxide solution (1mol/l.), 5.0mL of water and 20mL of glycerol, mix and shake well. 5.4.1.5 Lead standard stock solution: Weigh 0.1598g of lead nitrate, place in a 1000mL volumetric flask, add 5mL of nitric acid, dissolve with 50mL of water, dilute with water to the mark, and shake well.
5.4.1.6 Lead standard solution: Before use, accurately measure 10mL of the stock solution (5.4.1.5), place in a 100mL volumetric flask, dilute with water to the mark, and shake well.
5.4.2 Determination method
5.4.2.1 Method 1
Take 1g of this product and determine according to GB8451.
5.4.2.2 Method 2
Take 1g of this product, add 2mL of hydrochloric acid solution and water to make 25mL, dissolve with slight heat, cool to room temperature, and check according to Method 1 on page 52 of Appendix II of the 1990 edition of the Pharmacopoeia of the People's Republic of China. 5.4.2.3 Arbitration method: the first method.
5.5 Determination of loss on drying
5.5.1 Instruments and equipment
Constant temperature drying oven.
5.5.2 Determination method
Take this product according to the Appendix 55 of the 1990 edition of the Pharmacopoeia of the People's Republic of China, Part II, and dry it at 80℃ for 2 hours. The weight loss shall not exceed 277
5.5.3 Expression of analysis results
GB15571-1995
The loss on drying of the sample (X,) is expressed as a mass percentage and is calculated according to formula (2): X, = ma=ms × 100
Where: m3—mass of the sample and the weighing bottle before drying, g; m.—mass of the sample and the weighing bottle after drying, g; m2—mass of the sample, g.
5.6 Determination of sucrose or reducing sugar
5.6.1 Reagents and solutions
5.6.1.1 Hydrochloric acid (GB 622) solution: 3 mol/L. 5.6.1.2 Sodium carbonate test solution: Take 12.5 g of monohydrated sodium carbonate or 10.5 g of anhydrous sodium carbonate and add water to dissolve it into 100 mL. 5.6.1.3 Alkaline copper tartrate test solution:
(2)
Take 6.93 g of copper sulfate crystals and add water to dissolve it into 100 mL; a.
b, take 34.6g and 10g of sodium hydroxide, add water to dissolve into 100mL, mix the two liquids in equal amounts when using. 5.6.2 Determination method
Take 0.5g of this product, add 10mL of water and heat to dissolve, add 2mL of hydrochloric acid solution, boil for 2min, let it cool to room temperature, add 5mL of sodium carbonate test solution, let it stand for 5min, dilute with water to 20mL, filter; take 5mL of the filtrate, add 2mL of alkaline copper tartrate test solution, boil for 1min, and no red precipitate should be produced immediately.
5.7 Determination of chloride
5.7.1 Reagents and solutions
5.7.1.1 Nitric acid (GB626) solution: 9.5%~10.5%. 5.7.1.2 Silver nitrate (GB 670) solution: 0.1 mol/L. 5.7.1.3 Chloride standard solution: Weigh 0.165g of sodium fluoride, place in a 1000mL volumetric flask, add appropriate amount of water to dissolve, dilute to scale, shake well, and make a stock solution. Before use, accurately measure 10mL of the stock solution, place in a 100mL volumetric flask, dilute to scale with water, shake well, each milliliter is equivalent to 10 μg of Cl.
5.7.2 Determination method
Take 1g of this product and dissolve it in water to make 100mL, measure 10mL, and check according to page 48 of Appendix II of the 1990 edition of the Pharmacopoeia of the People's Republic of China. If turbidity occurs, its turbidity shall be compared with that of the control solution made of 5mL of standard sodium chloride solution, and shall not be darker (0.05%). 5.8 Determination of sulfate
5.8.1 Reagents and solutions
5.8.1.1 Hydrochloric acid (GB622) solution: 3mol/L. 5.8.1.2 Chloride (GB652) solution: 25%. 5.8.1.3 Standard potassium sulfate solution: Weigh 0.181g potassium sulfate, place in a 1000mL volumetric flask, add appropriate amount of water to dissolve and dilute to the scale and stir evenly, each milliliter is equivalent to 100μg SO4. 5.8.2 Determination method
Take 0.5g of this product, add water and dissolve it into about 40mL with slight heat, and check according to page 43 of Appendix II of the 1990 edition of the Pharmacopoeia of the People's Republic of China. If turbidity occurs, compare it with the control solution made of 2.5mL of standard potassium sulfate solution, and it shall not be darker (0.05%). 5.9 Determination of pH: Take 1.0g of this product, add 20mL of water to dissolve, and the pH value of the solution is 6.0~8.0. 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 batch of products shipped out of the factory shall be accompanied by a product inspection certificate. 278
GB 15571—1995
6.2 The user unit may conduct quality inspection on the received products in accordance with the inspection regulations and inspection methods specified in this standard to check whether its 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 a number of pieces. When the total number of pieces n≤3, each piece is sampled. When the total number of pieces is n≤300, the sampling number is /n+1. When the total number of pieces n>300, the sampling number is one + 1; take equal samples from each piece. After the samples are mixed evenly, use the quartering method to reduce the sample to 6 times the amount of the test, divide it into two parts and put it into 2
clean containers, affix labels, one for inspection and analysis, and the other sealed and preserved as a 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 verification. If there is still one indicator that does not meet the standard, 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 marked with the words "food additives", standard number, serial number, registered trademark, gross weight, net weight, batch number, factory name, factory address, and the barrel should contain the finished product inspection certificate. 7.2 This product is packed in two layers of polyethylene plastic bags and packaged in cardboard drums or iron drums. The packaging should meet the requirements of transportation and storage. 7.3 It should not be mixed with harmful substances during transportation, and should be prevented from heavy pressure, collision, exposure to the sun and rain. 7.4 This product should be stored in a dark place. , dry, fireproof, heatproof and moistureproof place, and shall not be stored together with toxic substances. 7.5 The shelf life of this product is four years under the original packaging conditions. Additional remarks:
This standard is proposed by the China Food and Drug Administration. This standard is jointly drafted and technically coordinated by China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. This standard is drafted by Shandong Xinhua Pharmaceutical Factory. The main drafter of this standard is Ye Yongdi.
This standard is not equivalent to the fifth edition of the Japanese Food Additive Code (1986). 2794 This product should be stored in a dark, dry, fireproof, heatproof and moistureproof place, and should not be mixed with toxic substances. 7.5 The shelf life of this product is four years under the original packaging conditions. Additional remarks:
This standard is proposed by the China Food and Drug Administration. This standard is jointly drafted and technically coordinated by China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. This standard is drafted by Shandong Xinhua Pharmaceutical Factory. The main drafter of this standard is Ye Yongdi.
This standard is not equivalent to the fifth edition of the Japanese Food Additive Code (1986). 2794 This product should be stored in a dark, dry, fireproof, heatproof and moistureproof place, and should not be mixed with toxic substances. 7.5 The shelf life of this product is four years under the original packaging conditions. Additional remarks:
This standard is proposed by the China Food and Drug Administration. This standard is jointly drafted and technically coordinated by China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. This standard is drafted by Shandong Xinhua Pharmaceutical Factory. The main drafter of this standard is Ye Yongdi.
This standard is not equivalent to the fifth edition of the Japanese Food Additive Code (1986). 279
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