GB 1903.53-2021National food safety standard - Food Nutrient Fortifier - D-calcium pantothenate (English PDF)

2.1 Chemical name

D-(+)-N-(2,4-dihydroxy-3,3-dimethylbutyryl)-beta-alanine calcium

2.2 Molecular formula

C18H32CaN2O10

2.3 structural formula

2.4 Relative molecular mass

476.54 (according to the international relative atomic mass in 2018)

3.1 Sensory requirements

Sensory requirements shall be in accordance with Table 1.

Appendix A

Inspection methods

A.1 General provisions

The reagents and water used in this Standard refer to analytical reagents and grade-3 water that is specified in GB/T 6682, when other requirements are not indicated. The standard solution, the standard solutions, preparations and products for impurity determination, which are used in the test, are all prepared in accordance with the provisions of GB/T 601, GB/T 602, and GB/T 603, when no other requirements are specified. The solution used in the test, if not indicated which solvent is used, refers to aqueous solution.

A.2 Identification test

A.2.1 Reagents and materials

A.2.1.1 Sodium hydroxide solution

43 g/L.

A.2.1.2 Copper sulfate solution

125 g/L.

A.2.1.3 Phenolphthalein indicator solution

10 g/L.

A.2.1.4 Hydrochloric acid solution

c(HCl) = 1 mol/L.

A.2.1.5 Ferric trichloride solution

90 g/L.

A.2.1.6 Ammonium oxalate solution

35 g/L.

A.2.1.7 Glacial acetic acid.

A.2.1.8 Hydrochloric acid.

A.2.1.9 Potassium bromide

spectrally pure, dry product.

A.2.2 Identification method

A.2.2.1 Weigh about 50 mg of the sample; add 5 mL of sodium hydroxide solution (A.2.1.1); shake; add 2 drops of copper sulfate solution (A.2.1.2), and it appears blue-purple.

A.2.2.2 Weigh about 50 mg of the sample; add 5 mL of sodium hydroxide solution (A.2.1.1); shake; boil for 1 min; let cool; add 1 drop of phenolphthalein indicator solution (A.2.1.3); add hydrochloric acid solution (A.2.1.4) until the solution fades; then, add another 0.5 mL of hydrochloric acid solution (A.2.1.4);

add 2 drops of ferric trichloride solution (A.2.1.5), and it appears bright yellow.

A.2.2.3 The identification reaction of the calcium salt in the aqueous solution of this product: Weigh 0.5 g of the sample; add 5 mL of water to dissolve; add ammonium oxalate solution (A.2.1.6), and a white precipitate appears; the precipitate is insoluble in glacial acetic acid; but it is soluble in hydrochloric acid.

A.2.2.4 Infrared spectroscopy

use potassium bromide pellet technique, to test according to GB/T 6040. The infrared spectrum of the sample shall be consistent with the infrared spectrum of the D-calcium pantothenate standard.

Refer to Figure B.1 in Appendix B for the standard infrared spectrum of D- calcium pantothenate.

A.2.2.5 Clarity

Weigh about 1.00 g of the sample; add 20 mL of water to dissolve; the solution is clear and colorless.

A.2.2.6 Solubility

easily soluble in water and glycerin; slightly soluble in ethanol;

insoluble in trichloromethane or ether.

A.3 Determination of D-calcium pantothenate content (on a dry basis)

A.3.1 Method summary

Use high performance liquid chromatography for determination, C18 chromatographic column for separation, UV detector for detection, and the peak area external standard method to quantitatively calculate the content of D- calcium pantothenate in the sample.

A.3.2 Reagents and materials

A.3.2.1 Acetonitrile

chromatographically pure.

A.3.2.2 Disodium hydrogen phosphate.

A.3.2.3 Sodium hydroxide solution

43 g/L.

A.3.2.4 Sodium dihydrogen phosphate solution

Weigh 3.2 g of sodium dihydrogen phosphate (A.3.2.2) into a 1 L volumetric flask; use water to dilute to the mark; mix well. Use sodium hydroxide solution (A.3.2.3) to adjust pH to

5.5.

A.3.2.5 D-sodium pantoate (CAS

60979-68-2): content >=97.0%.

A.3.2.6 D-calcium pantothenate standard (CAS

137-08-6): content >=99.0%.

A.3.3 Instruments and apparatuses

A.4.2.2 Ethylene Diamine Tetraacetic Acid standard titration solution: c(EDTA)

= 0.05 mol/L.

A.4.2.3 Calcium purpurin indicator

Take 0.1 g of calcium purpurin; add 10 g of anhydrous sodium sulfate; grind evenly, to get it.

A.4.3 Analysis steps

Weigh 0.5 g of the sample (accurate to 0.000 1 g); add 100 mL of water to dissolve; add 15 mL of sodium hydroxide solution (A.4.2.1) and about 0.1 g of calcium purpurin indicator (A.4.2.3); use Ethylene Diamine Tetraacetic Acid standard titration solution (A.4.2.2) to titrate, until the solution turns from purple to pure-blue.

A.4.4 Calculation results

The mass fraction w2 of calcium content (on a dry basis) is calculated according to Formula (A.2).

Where:

V2 - the volume of the Ethylene Diamine Tetraacetic Acid standard titration solution that is consumed by the sample solution, in milliliters (mL);

c3 - the concentration of the Ethylene Diamine Tetraacetic Acid standard titration solution, in moles per liter (mol/L);

M - the molar mass of calcium, in grams per mole (g/mol), M(Ca) = 40.08;

m2 - mass of the sample, in grams (g);

X3 - loss on drying of the sample, mass fraction, %.

Express the calculation result to one decimal place. The absolute difference of two independent test results under repeatability cannot exceed 0.6% of the arithmetic mean value.

A.5 Determination of specific rotation

A.5.1 Instruments and apparatuses

A.5.1.1 Polarimeter.

A.5.1.2 Polarimetry tube.

A.5.2 Analysis steps

potassium mercuric iodide test solution (A.7.1.2); leave it for 1 min; if there is no turbidity, it means that it passes the test.

A.8 Determination of alkalinity

A.8.1 Reagents and materials

A.8.1.1 Hydrochloric acid solution

0.1 mol/L.

A.8.1.2 Phenolphthalein indicator solution

10 g/L.

A.8.2 Analysis steps

Weigh about 1.0 g of the sample (accurate to 0.01 g); add 20 mL of carbon dioxide-free water to dissolve; immediately add 1 mL of hydrochloric acid solution (A.8.1.1) and 0.05 mL of phenolphthalein indicator solution (A.8.1.2); if there is no pink color within 5 s, the test is passed.

A.9 Determination of loss on drying

Weigh 2.0 g ~ 5.0 g of the sample (accurate to 0.000 1 g); the following operations are the same as the Method 1 of GB 5009.3-2016.

A.10 Determination of chloride

A.10.1 Reagents and materials

A.10.1.1 Nitric acid

A.10.1.2 Hydrochloric acid standard titration solution

0.001 4 mol/L.

A.10.1.3 Nitric acid solution

Take 105 mL of nitric acid (A.10.1.1); add water to dilute to 1 000 mL; shake well.

A.10.1.4 Silver nitrate solution

0.1 mol/L.

A.10.2 Analysis steps

Weigh about 2.5 g of the sample (accurate to 0.000 1 g) into a 50 mL volumetric flask; add 30 mL of boiling water to dissolve; dilute to the mark, as the test liquid.

Take 5 mL of the test solution; add 10 mL of boiled water; add 6 mL of nitric acid solution (A.10.1.3); mix well, pour the mixed solution into a colorimetric tube that contains 1 mL of silver nitrate solution (A.10.1.4); shake well, as the sample solution. Take another 1 mL of hydrochloric acid standard titration solution (A.10.1.2); add 14 mL of boiled water; add 6 mL of nitric acid solution (A.10.1.3);

mix well; pour the mixed solution into a colorimetric tube that contains 1 mL of silver nitrate solution (A.10.1.4); shake well, as the control solution. After placing

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