Some standard content:
National Standard of the People's Republic of China
Food additive--Folic acid
Subject content and scope of application
GB15570--1995
This standard specifies the technical requirements, test methods, inspection rules and requirements for marking, packaging, transportation and storage of folic acid, a food additive. This standard applies to folic acid obtained by chemical synthesis, which is used as a vitamin substitute and fortifier in the food industry. 2 Reference Standards
Pharmacopoeia of the People's Republic of China: Part II of the 1990 edition GB8450 Determination of metals in food additives GB8451 Limit test method for heavy metals in food additives 3 Chemical name, molecular formula, structural formula, molecular weight Chemical name: N-[4-[(2-Amino-1, 4-dihydro-4-oxo-6-pteridinyl)methylamino]benzoyl]-1.-glutamic acid N-[4-[(2-Amino-1, 4-dihydro-4-oxo-6-pteridinyl)methylamino]benzoyl]-1.-glutamic acid JL-glutamicAcid
Molecular formula: CrgH1N,O6
Structural formula:
HOOCCH,CH2-
Molecular weight: 441.40 (according to the international atomic weight in 1987) 4 Technical requirements
4.1 Properties
This product is yellow or orange-yellow crystalline powder; odorless and tasteless. Insoluble in water, ethanol, acetone, chloroform or ether; soluble in dilute solutions of sodium hydroxide and sodium carbonate.
4.2 Items and indicators
Approved by the State Bureau of Technical Supervision on June 2, 1995, and implemented on December 1, 1995
Content (as Chlorine, Hydrogen, Nitrogen, Oxide), %
Minerals, %
Residue on ignition, %
Heavy metals (as Pb), %
Arsenic (as As), %
5 Test method
GB15570--1995
96.0～102.0 (First method)
95.0～102.0 (Second method)
The reagents used in the tests of this standard are analytically pure reagents, water is distilled water or water of corresponding purity, and the solution is an aqueous solution. 5.1 Identification
5.1.1 Reagents and solutions
Sodium hydroxide (GB629): 0.1 mol/L solution. 5.1.2 Instruments and equipment
Ultraviolet spectrophotometer with 1 cm colorimetric cell. 5.1.3 Identification method
Take a sample, add sodium hydroxide solution to make a solution containing 10ug of sample per 1mL, and measure it with an ultraviolet spectrophotometer. The maximum absorption is at the wavelengths of 256±2nm, 283±2nm, and 365±4nm. The ratio of the absorbance at 256nm to the absorbance at 365nm should be 2.8~～3.0.
5.2 Determination of folic acid content
5.2.1 The first method of colorimetric spectrometry
5.2.1.1 Reagents and solutions
Sodium hydroxide (GB629): 0.1 mol/L solution. Hydrochloric acid (GB622): 2mol/L solution.
Zinc powder (arsenic-free zinc).
Sodium nitrite (GB633): 0.1% solution. Ammonium sulfamate: 0.5% solution.
Naphthylethylenediamine dihydrochloride: 0.1% solution. Preparation of reference solution: Weigh 0.08g (accurate to 0.0002g) of folic acid reference (water content is determined simultaneously), place in a 100mL volumetric flask, add sodium hydroxide solution to dissolve, dilute to scale, and shake well (solution A). Accurately pipette 2mL of solution A, place in another 100mL volumetric flask, add 20mL of hydrochloric acid solution, dilute to scale with water, shake well, and obtain. Each 1mL contains about 16μg of folic acid reference (solution B). Preparation of sample solution: Weigh the folic acid sample and prepare it according to the preparation method of the reference solution. 5.2.1.2 Instruments and equipment
Spectrophotometer with 1 cm colorimetric cell.
5.2.1.3 Determination method
Precisely measure 60 mL of reference solution B and sample solution B, respectively, and place them in 250 mL stoppered conical flasks, add 0.5 g of zinc powder to each (a little excess is acceptable), shake continuously for 20 min, filter with dry filter paper, discard the primary filtrate, accurately take 2 mL of the subsequent filtrate, place them in 10 mL volumetric flasks, add 3 mL of water, 1 mL of hydrochloric acid solution and 1 mL of sodium nitrite, mix well, let stand for 2 min, add 1 mL of ammonium sulfamate solution to each, mix well, let stand for 10 min, add 1 mL of naphthylethylenediamine dihydrochloride solution to each, mix well, let stand for 10 min, dilute to the mark with water, and spread evenly. 270
GB15570—1995
Precisely pipette 20mL of reference solution A and sample solution A respectively, place them in 100mL volumetric flasks, add 20mL of hydrochloric acid solution to each, dilute to scale with water, and shake well. Precisely pipette 2mL of each, place them in 10mL volumetric flasks respectively, and operate according to the procedure starting from “add 3mL of water in sequence”; take another 2mL of water and place it in an 18L volumetric flask, and operate according to the procedure starting from “add 3mL of water in sequence” as blank, and measure with a spectrophotometer, and measure the absorbance of the above two groups of solutions at a measured length of 550±1 am with a 1 cm colorimetric cell. 5.2.1.4 Expression of calculation results
Folic acid content X, (expressed as mass percentage) is calculated according to formula (1): x - % = 48:0 (88-%
Absorbance of reference solution reduced with zinc powder; Wherein: A,
A2——absorbance of sample solution reduced with zinc powder; A: absorbance of reference solution not reduced with zinc powder; A.absorbance of sample solution not reduced with zinc powder, ml—mass of reference, g;
m2 mass of sample, g.
X,——water content of reference, %,
X.-——water content of sample, %.
Note: X2, X, are as per 5.3 Determination.
5.2.1.5 Allowable error
The relative deviation of two parallel tests should be less than 2%. 5.2.2 Second method High performance liquid chromatography
5.2.2.1 Reagents
Potassium dihydrogen phosphate (GB1274).
Potassium hydroxide (HGB3006): 0.1 mol/L solution in methanol (HPLC chromatography grade).
Nicotinamide (pharmaceutical grade).
Ammonia water (GB631): 0.5% solution.
Folic acid reference substance (Institute for the Identification of Biological Products, Ministry of Health of China). 5.2.2.2 Instruments
High performance liquid chromatograph with octadecylsilane bonded silica gel column. 5.2.2.3 System suitability test
...(1)
Use 6.8 g of potassium dihydrogen phosphate and 70% potassium hydroxide solution (0.1 mol/L) to obtain a chromatographic column. mL, dilute with water to about 850 mL and adjust the pH to 6.3 ± 0.1, add 80 mL of methanol, dilute with water to 1000 mL of solution as the mobile phase; the detection wavelength is 254 nm, and the separation degree of folic acid peak and internal standard substance peak should be greater than 1.5.
The separation degree (R) is calculated according to formula (2): wwW.bzxz.Net
2(tk, - tr,)
W.---the width of the folic acid peak;
-the width of the nicotinamide peak.
5.2.2.4 Determination of correction factor
GB 15570-1995
Take an appropriate amount of nicotinamide, dissolve it in water and dilute it to 1 mL containing 1. 0mg solution as internal standard solution. Weigh 5mg folic acid reference substance (accurate to 0.00002g) and place it in a 25mL volumetric flask. Add about 15mL of 0.5% ammonia solution to dissolve it. Accurately add 5mL of internal standard solution, dilute to scale with the same solvent, shake, take 10 μl and inject it into the liquid chromatograph to calculate the correction factor. The correction factor (F,) is calculated according to formula (3):
Where: As——2
The peak area of nicotinamide;
A. -——-The peak area of folic acid reference substance; m3-
The mass of nicotinamide, g;
The mass of folic acid reference substance, g.
5.2.2.5 Preparation and determination of test solution As/ma
Take about 5mg of this product (accurate to 0.00002g) and prepare and determine the folic acid reference substance solution according to the correction factor determination item in 5.2.2.4.
5.2.2.6 Expression of calculation results
Folic acid content X (expressed as mass percentage) is calculated according to formula (4): A./ms×100
X4=F×
Wherein, F,
Correction factor,
Folic acid peak area;
A:——Nicotinamide peak area;
The mass of a sample, g;
Nicotinamide mass, g.
5.2.2.7 Allowable difference
The relative deviation of two parallel tests should be less than 2%. 5.3 Determination of moisture
5.3.1 Reagents
Fischer's test solution: Preparation method and calibration shall be in accordance with page 55 of Appendix II of the Pharmacopoeia of the People's Republic of China, 1999 edition. Anhydrous methanol (analytical grade).
Trichloromethane (GB682).
5.3.2 Instruments and equipment
Fischer's moisture meter.
5.3.3 Determination method
Weigh 0.1g of sample (accurate to 0.0002g), place in a dry stoppered glass bottle, add 5mL of chloroform and anhydrous methanol (4:1), and titrate with Fischer's test solution under continuous shaking (or stirring) until the solution changes from light yellow to reddish brown. Perform a blank test in the same way. 5.3.4 Expression of calculation results
The water content X in the sample (expressed as mass percentage) is calculated according to formula (5): 272
GB 15570—1995
(Ti- T2)·F2
Where: F -- the mass of water equivalent to 1mL of Fischer's test solution, mgTi The volume of Fischer's test solution consumed by the sample, mL, T.
The volume of Fischer's test solution consumed by the blank, mL The mass of the sample, mg.
5.3.5 Allowable difference
The relative deviation of two parallel tests should be less than 0.2%. 5.4 Determination of ignition residue
5.4.1 Reagents
Sulfuric acid (GB 625).
5.4.2 Determination method
Weigh 1g of sample (accurate to 0.01g) and place it in a porcelain pot that has been ignited at 700-800℃ to constant weight. Heat slowly over low heat until it is completely carbonized. After cooling, add 0.5~~1mL of sulfuric acid to moisten it. Heat at low temperature until sulfuric acid vapor is completely removed, and then ignite at 700-800℃ to constant weight. 5.4.3 Expression of calculation results
Ignition residue X. (expressed as mass percentage) Calculate according to formula (6): X, = mo2m × 100
Where: mg plus residue mass, g;
mg-crumb mass, g;
-sample mass, nom.
5.5 Determination of heavy metals
5.5.1 Method 1
Determine according to GB8451, and the sample is treated by dry digestion. This method is the arbitration method. 5.5.2 Method 2
Operate according to method 5.4.2 (but burn at 500-600℃), and check according to Method 2 on page 52 of Appendix II of the 1990 edition of the Pharmacopoeia of the People's Republic of China.
5.6 Determination of arsenic
Determine according to GB8450, and the sample is treated by dry ashing method under the diethylaminodithiocarbamate silver colorimetric method. 6 Inspection rules
6.1 This product should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all products leaving the factory meet the requirements of this standard. Each batch (piece) of products leaving the factory should be accompanied by a product inspection certificate. 6.2 The user can conduct quality inspection on the received products according to 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
For sampling, clean, dry, airtight and light-proof sample bottles must be prepared. The bottles shall be labeled with the manufacturer name, product name, batch number and sampling date. Each package is one piece. The total number of pieces n≤3. The sampling number is each piece. When the total number of pieces n≤300, the sampling number is n
/n+1; when the total number of pieces n>300, the sampling number is
+1. An equal amount of samples are taken from each piece and the sampling is reduced by quartering. Two samples are taken from each batch of products. The sample size of each sample should be 3 times the amount of the sample required for inspection and placed in a sample bottle. One sample is sent to the laboratory for inspection and the other is sealed and kept for arbitration analysis. 6.5 If one of the indicators does not meet the standard during the inspection, a new sample should be taken from more than twice the amount of packaging for verification. If the product re-inspection result shows that only one indicator does not meet the standard, the batch is unqualified. 6.6 If the supply and demand parties have objections to the product quality, the statutory arbitration unit may conduct arbitration acceptance according to the acceptance regulations and inspection methods of this standard.
7 Marking, packaging, transportation and storage
7.1 The packaging should have firm and clear markings, including: product name, factory name, factory address, approval number, trademark, production date, batch number, net weight, quality grade, shelf life, etc.
7.2 The inner packaging of this product is a double-layer polyethylene film bag, which is sealed, and the outer packaging is a tin barrel or cardboard barrel. 7.3 During transportation, it should be avoided from sun, rain, heat and impact. It should be handled with care and not mixed with toxic, harmful or other contaminated items.
7.4 This product should be stored in a cool and dry place. 7.5 The shelf life of this product is three years under the original packaging conditions. Additional remarks:
This standard was proposed by the State Drug Administration and organized by China Pharmaceutical Industry Corporation. This standard is under the jurisdiction of the Tianjin Pharmaceutical Research Institute of the State Drug Administration. This standard was drafted by Changzhou Pharmaceutical Factory. The main drafters of this standard are He Jiaying, Zhang Chunhua and Xu Ruiqun. This standard is not equivalent to the US Food Chemical Codex FCC1983 (1). 2742 The user can conduct quality inspection on the received products according to the inspection rules and test methods specified in this standard to check whether their indicators meet the requirements of this standard.
6.3 The finished products with uniformity after the final mixing are considered as one batch. 6.4 Sampling method and sampling quantity
For sampling, clean, dry, airtight and light-proof sample bottles must be prepared. The bottles shall be labeled with the manufacturer name, product name, batch number and sampling date. Each package is one piece. The total number of pieces n≤3. The sampling number is each piece. When the total number of pieces n≤300, the sampling number is n
/n+1; when the total number of pieces n>300, the sampling number is
+1. An equal amount of samples are taken from each piece and the sampling is reduced by quartering. Two samples are taken from each batch of products. The sample size of each sample should be 3 times the amount of the sample required for inspection and placed in a sample bottle. One sample is sent to the laboratory for inspection and the other is sealed and kept for arbitration analysis. 6.5 If one of the indicators does not meet the standard during the inspection, a new sample should be taken from more than twice the amount of packaging for verification. If the product re-inspection result shows that only one indicator does not meet the standard, the batch is unqualified. 6.6 If the supply and demand parties have objections to the product quality, the statutory arbitration unit may conduct arbitration acceptance according to the acceptance regulations and inspection methods of this standard.
7 Marking, packaging, transportation and storage
7.1 The packaging should have firm and clear markings, including: product name, factory name, factory address, approval number, trademark, production date, batch number, net weight, quality grade, shelf life, etc.
7.2 The inner packaging of this product is a double-layer polyethylene film bag, which is sealed, and the outer packaging is a tin barrel or cardboard barrel. 7.3 During transportation, it should be avoided from sun, rain, heat and impact. It should be handled with care and not mixed with toxic, harmful or other contaminated items.
7.4 This product should be stored in a cool and dry place. 7.5 The shelf life of this product is three years under the original packaging conditions. Additional remarks:
This standard was proposed by the State Drug Administration and organized by China Pharmaceutical Industry Corporation. This standard is under the jurisdiction of the Tianjin Pharmaceutical Research Institute of the State Drug Administration. This standard was drafted by Changzhou Pharmaceutical Factory. The main drafters of this standard are He Jiaying, Zhang Chunhua and Xu Ruiqun. This standard is not equivalent to the US Food Chemical Codex FCC1983 (1). 2742 The user can conduct quality inspection on the received products according to the inspection rules and test methods specified in this standard to check whether their indicators meet the requirements of this standard.
6.3 The finished products with uniformity after the final mixing are considered as one batch. 6.4 Sampling method and sampling quantity
For sampling, clean, dry, airtight and light-proof sample bottles must be prepared. The bottles shall be labeled with the manufacturer name, product name, batch number and sampling date. Each package is one piece. The total number of pieces n≤3. The sampling number is each piece. When the total number of pieces n≤300, the sampling number is n
/n+1; when the total number of pieces n>300, the sampling number is
+1. An equal amount of samples are taken from each piece and the sampling is reduced by quartering. Two samples are taken from each batch of products. The sample size of each sample should be 3 times the amount of the sample required for inspection and placed in a sample bottle. One sample is sent to the laboratory for inspection and the other is sealed and kept for arbitration analysis. 6.5 If one of the indicators does not meet the standard during the inspection, a new sample should be taken from more than twice the amount of packaging for verification. If the product re-inspection result shows that only one indicator does not meet the standard, the batch is unqualified. 6.6 If the supply and demand parties have objections to the product quality, the statutory arbitration unit may conduct arbitration acceptance according to the acceptance regulations and inspection methods of this standard.
7 Marking, packaging, transportation and storage
7.1 The packaging should have firm and clear markings, including: product name, factory name, factory address, approval number, trademark, production date, batch number, net weight, quality grade, shelf life, etc.
7.2 The inner packaging of this product is a double-layer polyethylene film bag, which is sealed, and the outer packaging is a tin barrel or cardboard barrel. 7.3 During transportation, it should be avoided from sun, rain, heat and impact. It should be handled with care and not mixed with toxic, harmful or other contaminated items.
7.4 This product should be stored in a cool and dry place. 7.5 The shelf life of this product is three years under the original packaging conditions. Additional remarks:
This standard was proposed by the State Drug Administration and organized by China Pharmaceutical Industry Corporation. This standard is under the jurisdiction of the Tianjin Pharmaceutical Research Institute of the State Drug Administration. This standard was drafted by Changzhou Pharmaceutical Factory. The main drafters of this standard are He Jiaying, Zhang Chunhua and Xu Ruiqun. This standard is not equivalent to the US Food Chemical Codex FCC1983 (1). 274
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