GB 1903.45-2020 English PDF (GB1903.45-2020)

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GB 1903.45-2020: National food safety standard - Food Nutritional Fortification Substance - Nicotinamide
GB 1903.45-2020
National food safety standard-Food nutritional fortification substance-Nicotinamide
National Standards of People's Republic of China
National Food Safety Standard
Food nutrition fortifier nicotinamide
2020-09-11 released
2021-03-11 implementation
National Health Commission of the People's Republic of China
Issued by the State Administration for Market Regulation
National Food Safety Standard
Food nutrition fortifier nicotinamide
1 Scope
This standard applies to methyl nicotinate (or ethyl nicotinate, or 3-methylpyridine, or 3-cyanopyridine, or 2-methyl-1,5-pentanediamine) as the original
It is a food nutrient fortifier nicotinamide produced through the corresponding chemical synthesis process.
2 Chemical name, structural formula, molecular formula and relative molecular mass
2.1 Chemical name
3-pyridine carboxamide
2.2 Structural formula
2.3 Molecular formula
C6H6N2O
2.4 Relative molecular mass
122.13 (according to.2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements should meet the requirements of Table 1.
3.2 Physical and chemical indicators
The physical and chemical indicators should meet the requirements of Table 2.
Appendix A
Testing method
A.1 General provisions
When the reagents and water used in this standard are not specified other requirements, they all refer to the analytical reagents and the tertiary water specified in GB/T 6682.Testing
The standard solutions used, standard solutions for impurity determination, preparations and products are in accordance with GB/T 601, GB/T 602,
Prepared according to GB/T 603.The solution used in the test refers to an aqueous solution when it is not specified which solvent is used for preparation.
A.2 Identification test
A.2.1 Color reaction
A.2.1.1 Reagents and materials
A.2.1.1.1 Sodium hydroxide solution. Weigh 4.3g of sodium hydroxide, add 100mL of water, stir to dissolve and mix.
A.2.1.1.2 Phenolphthalein indicator solution.
A.2.1.1.3 Sulfuric acid solution. Measure 57mL sulfuric acid, slowly add to water, and dilute to 1000mL with water, and mix.
A.2.1.1.4 Copper sulfate solution. Weigh 12.5g copper sulfate pentahydrate, add 100mL water, stir to dissolve and mix.
A.2.1.2 Analysis steps
Weigh 0.1g sample (accurate to 0.01g), add 5mL water to dissolve, add 5mL sodium hydroxide solution, and slowly heat, it should produce ammonia and
Make the wet red litmus paper blue (the difference from niacin). Continue to heat until the ammonia odor is completely removed, let it cool, and add 1 to 2 drops of phenolphthalein to indicate
Liquid, neutralize with sulfuric acid solution, add 2mL copper sulfate solution, a light blue precipitate should slowly precipitate.
A.2.2 Infrared spectrum test
Use potassium bromide tablet method to test in accordance with GB/T 6040.The infrared spectrum of the sample should be the same as that of the nicotinamide standard.
Consistent (see Figure B.1 for the infrared spectrum of the nicotinamide standard).
A.2.3 UV absorption
A.2.3.1 Instruments and equipment
UV spectrophotometer.
A.2.3.2 Preparation of sample solution
Weigh 0.1g of the sample (accurate to 0.01g), dissolve it with distilled water and dilute to 100mL, shake it well, draw 2.00mL of the solution, and distill
Dilute with water and dilute to 100mL, shake well, and use as a sample solution for later use.
A.2.3.3 Analysis steps
Pour the sample solution (A.2.3.2) into a 1cm quartz cuvette, and measure the absorbance at 261nm and 245nm with distilled water as a blank
Degree, there should be a maximum absorption value at 261nm wavelength, and a minimum absorption value at 245nm wavelength.
A.3 Determination of nicotinamide content (on a dry basis)
A.3.1 Reagents and materials
A.3.1.1 Perchloric acid (HClO4). pure superior grade.
A.3.1.2 Perchloric acid standard titration solution. c(HClO4)=0.1mol/L.
A.3.1.3 Glacial acetic acid.
A.3.1.4 Water. Grade 1 water specified in GB/T 6682.
A.3.1.5 5g/L crystal violet indicator solution. Weigh 0.5g of crystal violet, add 100mL of glacial acetic acid to dissolve it, and get it.
A.3.1.6 Methanol (CH3OH). chromatographically pure.
A.3.1.7 Isopropanol (C3H8O). chromatographically pure.
A.3.1.8 Sodium heptane sulfonate (C7H15NaO3S). chromatographically pure.
A.3.1.9 Nicotinamide (C6H6N2O) standard product. the mass score is greater than 99.0%, or the standard that has been certified by the country and awarded the certificate of reference material
substance.
A.3.2 Instruments and equipment
A.3.2.1 High performance liquid chromatograph with UV detector.
A.3.2.2 Potentiometric titrator.
A.3.2.3 Electronic balance. the accuracy is 0.0001g.
A.3.2.4 pH meter. the accuracy is 0.01.
A.3.3 Analysis steps
A.3.3.1 Perchloric acid titration method
A.3.3.1.1 Indicator titration method
A.3.3.1.1.1 Method summary
Using crystal violet as indicator, titrate the sample with perchloric acid standard solution, and calculate the nicotinamide content based on the amount of perchloric acid standard titrant.
A.3.3.1.1.2 Analysis steps
Weigh 0.1g sample (accurate to 0.0001g), add 30mL glacial acetic acid to dissolve (if necessary, slightly warm it to completely dissolve). plus
Add 1 to 2 drops of crystal violet indicator solution, titrate with perchloric acid standard titration solution until the solution turns blue-green, and the color does not fade within 30 seconds, that is, titration
end. Do a blank test at the same time.
A.3.3.1.2 Potentiometric titration method
A.3.3.1.2.1 Method summary
The calomel electrode was used as the reference electrode, and the non-aqueous acid-base titration glass electrode was used as the indicator electrode. The sample was titrated with perchloric acid standard solution. according to
The "jump" of the potential determines the end point of the titration. According to the amount of perchloric acid standard titrant, calculate the nicotinamide content.
A.3.3.1.2.2 Analysis steps
Weigh 0.1g sample (accurate to 0.0001g), add 30mL glacial acetic acid to dissolve it (if necessary, slightly warm it to dissolve completely; like ice
Acetic acid cannot flood the electrode, and glacial acetic acid can be added appropriately). Titrate with a perchloric acid standard titration solution with a potentiometric titrator, and do a blank test at the same time.
A.3.3.2 Liquid chromatography
A.3.3.2.1 Method summary
Dissolve the sample in water, separate it with a C18 chromatographic column, and detect it at a wavelength of 261nm with a UV detector, which is determined by the retention time of the chromatographic peak
The content of nicotinamide in the sample was calculated by the external standard method.
A.3.3.2.2 Reference conditions for liquid chromatography
The reference conditions are as follows.
a) Chromatographic column. C18 (particle size 5μm, 250mm×4.6mm), or a chromatographic column with equivalent performance.
b) Ultraviolet detector. detection wavelength is 261nm.
c) Mobile phase. Dissolve and mix 70 mL methanol, 20 mL isopropanol, and 1 g sodium heptane sulfonate with 910 mL of water, then use perchloric acid
Adjust the pH to 2.1±0.1 and filter through 0.45μm membrane.
d) Flow rate. 1.0mL/min.
e) Injection volume. 20μL.
f) Column temperature. room temperature.
A.3.3.2.3 Preparation of sample solution
Accurately weigh 0.1g sample (accurate to 0.0001g), place it in a 100mL volumetric flask, dissolve it with mobile phase and dilute to the mark, mix
Homogenize; then accurately pipet 10mL in a 100mL volumetric flask, add mobile phase to the volume and mix well, as a sample solution.
A.3.3.2.4 Preparation of standard solution
Accurately weigh 0.1g (accurate to 0.0001g) niacinamide standard, place it in a 100mL volumetric flask, dissolve it with mobile phase and dilute to
Scale and mix; then accurately pipette 10mL to 100mL volumetric flask, dilute to the mark with mobile phase, mix well, and use it as a standard solution.
A.3.3.2.5 Determination
According to the established chromatographic conditions, the nicotinamide standard solution and sample solution were injected into the liquid chromatography for determination. Record color
Spectral peak area.
A.3.4 Result calculation
A.3.4.1 Perchloric acid titration method
The mass fraction w1 of the content of nicotinamide in the sample (calculated on a dry basis) is calculated according to formula (A.1).
The test results are based on the arithmetic mean of the parallel determination results. Absolute difference between two independent determination results obtained under repeatability conditions
The value is not more than 0.5% of the arithmetic mean.
A.3.4.2 Liquid chromatography
The mass fraction w2 of the content of nicotinamide in the sample (calculated on a dry basis) is calculated according to formula (A.2).
The test results are based on the arithmetic mean of the parallel determination results. Absolute difference between two independent determination results obtained under repeatability conditions
The value is not more than 0.5% of the arithmetic mean.
A.4 Determination of absorption coefficient E1 m (261nm)
A.4.1 Principle of the method
The purity of the sample is expressed by measuring the absorption coefficient of the sample solution at a specific wavelength.
A.4.2 Reagents and materials
Hydrochloric acid solution. 0.1mol/L.
A.4.3 Instruments and equipment
A.4.3.1 1cm quartz cuvette.
A.4.3.2 UV spectrophotometer.
A.4.3.3 Electronic balance with an accuracy of 0.0001g.
A.4.4 Analysis steps
Accurately weigh 0.15g of the sample (accurate to 0.0001g), dilute to 100mL with hydrochloric acid solution, mix well; then measure 1.00mL in 100mL
In the volumetric flask, add the hydrochloric acid solution to the mark and mix well to form the sample solution. Pour the sample solution into a 1cm quartz cuvette and dissolve it with hydrochloric acid
The liquid is a reference liquid, and the absorption coefficient (E 1 m) is measured at a wavelength of 261 nm with a spectrophotometer.
A.4.5 Result calculation
The absorption coefficient E1 m is calculated according to formula (A.3).
The test results are based on the arithmetic mean of the parallel determination results. Absolute difference between two independent determination results obtained under repeatability conditions
The value is not more than 2% of the arithmetic mean.
A.5 Absorbance ratio
A.5.1 Instruments and equipment
UV spectrophotometer.
A.5.2 Analysis steps
The sample solution (A.2.3.2) was poured into a 1cm quartz cuvette, and the absorbance at the wavelength of 245nm and 261nm were measured respectively.
Note. The absorption peak wavelength should be within ±2nm of the specified wavelength, and the peaks and valleys appear as the measurement wavelength.
A.5.3 Result calculation
The UV absorbance ratio X is calculated according to formula (A.4).
The test results are based on the arithmetic mean of the parallel determination results. Absolute difference between two independent determination results obtained under repeatability conditions
The value is not more than 1% of the arithmetic mean.
A.6 Drying loss
A.6.1 Instruments and equipment
A.6.1.1 Vacuum drying oven.
A.6.1.2 Electronic balance with an accuracy of 0.0001g.
A.6.1.3 Weighing bottle.
A.6.2 Analysis steps
Weigh 1g of the sample (accurate to 0.0001g) and place it in a weighing bottle that is dried to a constant weight (the difference in weighing after two consecutive dryings is 0.3mg
In the following), the thickness is not more than 5mm, placed in a vacuum drying oven with phosphorus pentoxide as a desiccant. Exhaust the air in the vacuum drying oven,
The pressure was kept below 2.67kPa and maintained at room temperature for 18h. Take out the weighing bottle, close the bottle cap, put it in a desiccator and let it cool, and then weigh it
Quantity (accurate to 0.0001g). Calculate the loss on drying of the sample from the lost weight and the sample size.
Note. Under reduced pressure, the bottle cap should not be placed in a vacuum drying oven to avoid cracking.
A.6.3 Result calculation
The mass fraction w3 of loss on drying is calculated according to formula (A.5).
A.7 Clarity and color
A.7.1 Instruments and equipment
Electronic balance with an accuracy of 0.01g.
A.7.2 Analysis steps
Take 1g sample (accurate to 0.01g), add 10mL water to dissolve, the solution is clear and colorless to pass the test.
A.8 Easily charred
A.8.1 Method summary
The sample is dissolved in a sulfuric acid solution, and compared with the control solution, the color should not be darker.
A.8.2 Reagents and materials
A.8.2.1 Sulfuric acid.
A.8.2.2 Ammonia test solution. Measure 40mL of concentrated ammonia, add water to dilute to 100mL, and mix.
A.8.2.3 Hydrochloric acid. analytically pure.
A.8.2.4 Cobalt chloride solution for color comparison. Weigh 32.5g of cobalt chloride hexahydrate (CoCl2 6H2O) (accurate to 0.0001g), and add an appropriate amount of salt
Dissolve the acid solution (1→40) into 500mL, measure 2.00mL, place it in an Erlenmeyer flask, add.200mL water to mix, add ammonia solution to the solution
After changing from light red to green, add 10 mL of acetic acid-sodium acetate buffer (pH 6.0), heat to 60°C, and add 5 drops of xylenol orange to indicate dissolution
Solution, titrate with disodium ethylenediaminetetraacetic acid titration solution (0.05mol/L) to appear yellow. Per 1mL disodium edetate titration solution
(0.05mol/L) is equivalent to 11.90mg of cobalt chloride hexahydrate. According to the above measurement results, add an appropriate amount of hydrochloric acid solution to the remaining original solution
(1→40), so that each 1mL solution contains 59.5mg of cobalt chloride hexahydrate, which is obtained.
A.8.2.5 Potassium dichromate solution for color comparison. Weigh 0.4g of reference potassium dichromate (accurate to 0.0001g) dried at 120°C to constant weight, and place
In a 500mL volumetric flask, add an appropriate amount of water to dissolve and dilute to the mark, shake well, and it is ready. 0.800mg of dichromic acid per 1mL solution
Potassium (K2Cr2O7).
A.8.2.6 Copper sulfate solution for color comparison. Weigh 32.5g of copper su...