National Health Commission and State Administration for Market Regulation
Issued on:
2020-09-11
Implemented on:
2021-3-11
Status:
valid
Language:
English
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PDF
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5500 words
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Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
National food safety standard
Nutritional fortification substances in foods - Cholecalciferol (vitamin D3)
1 Scope
This standard is applicable to cholecalciferol (vitamin D3), a nutritional fortification substance in foods, which is prepared with lanolin cholesterol as raw material to obtain 7-dehydrocholesterol by chemical synthesis, ultraviolet irradiation and refining.
2 Chemical name, structural formula, molecular formula and relative molecular mass
2.1 Chemical name
(5Z,7E)-9,10-Secocholesta-5,7,10 (19)-triene-3β-ol
2.2 Structural formula
2.3 Molecular formula
C27H44O
2.4 Relative molecular mass
384.64 (according to the international relative atomic mass in 2018)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall meet those specified in Table 1.
Table 1 Sensory requirements
Item Requirement Inspection method
Color and luster Colorless or white Put a proper amount of sample into a clean and dry white porcelain dish, then observe its color and luster as well as state in natural light and smell it
Odor No odor or peculiar smell
State Acicular crystal or crystalline powder
3.2 Physical and chemical indexes
Physical and chemical indexes shall meet those specified in Table 2.
Table 2 Physical and chemical indexes
Item Index Inspection method
Content of vitamin D3, ω/% 97.0~103.0 A.3, Annex A
Specific rotation αm (20℃, D)/(°)·dm2·kg-1 +105.0~+112.0 A.4, Annex A
Absorption coefficient (265nm)
465~495 A.5, Annex A
Related substances: provitamin D3, trans-vitamin D3, tachysterol D3, 7-dehydrocholesterol Except for the peak of provitamin D3, the peak area of a single impurity shall not be greater than 0.5 times the main peak area of control solution; the sum of impurity peak areas shall not be greater than the main peak area of control solution A.6, Annex A
Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.75 or GB 5009.12
Total arsenic (by As)/(mg/kg) ≤ 2.0 GB 5009.76 or GB 5009.11
Note: Commercial products of cholecalciferol (vitamin D3) shall be made of cholecalciferol (vitamin D3) complying with this standard, and added with necessary food materials and/or food additives as auxiliary materials with the mass, range and consumption meeting the relevant requirements of corresponding national food safety standards.
Annex A
Inspection method
A.1 General requirements
Unless otherwise specified, analytically pure reagents or above and Class-III water specified in GB/T 6682 are adopted for the purposes of this standard. Unless otherwise specified, the standard solution used in the tests and the standard solution, preparations and products for determination of impurities are prepared in accordance with GB/T 601, GB/T 602 and GB/T 603. Unless otherwise specified, the solution used in the tests refers to the aqueous solution.
A.2 Identification test
A.2.1 Color reaction of acetic anhydride and concentrated sulfuric acid
A.2.1.1 Reagents and materials
A.2.1.1.1 Trichloromethane.
A.2.1.1.2 Acetic anhydride.
A.2.1.1.3 Sulfuric acid.
A.2.1.2 Identification method
Weigh 0.5mg sample, add 5mL trichloromethane to dissolve it, add 0.3mL acetic anhydride and 0.1mL sulfuric acid, shake it, it will turn yellow at first, gradually turn red, then turn purple and blue-green immediately, and finally turn green.
A.2.2 Infrared spectrum test
A.2.2.1 Reagents and materials
Potassium bromide.
A.2.2.2 Apparatus
Infrared spectrometer.
A.2.2.3 Analysis steps
Carry out test by potassium bromide pellet technique according to GB/T 6040, the infrared spectrum of the sample shall be consistent with the standard infrared spectrogram. See Figure B.1 for the standard infrared spectrogram of vitamin D3.
A.3 Determination of content of vitamin D3
A.3.1 Method summary
Determine vitamin D3 by high-performance liquid chromatography after dissolution and dilution, and calculate the content of vitamin D3 by external standard method.
A.3.2 Reagents and materials
A.3.2.1 n-hexane: chromatographically pure.
A.3.2.2 n-amyl alcohol: chromatographically pure.
A.3.2.3 Isooctane: chromatographically pure.
A.3.2.4 Vitamin D3 standard: with a mass fraction of not less than 98%.
A.3.2.5 7-dehydrocholesterol standard: with a mass fraction of not less than 98%.
A.3.2.6 Water: Class-I water complying with GB/T 6682.
A.3.3 Apparatus
High-performance liquid chromatograph: equipped with ultraviolet detector or equivalent detector.
A.3.4 Chromatography reference conditions
The recommended chromatographic column and typical chromatographic operating conditions are listed below; other chromatographic columns and chromatographic conditions which can reach the same separation may also be adopted.
A.3.4.1 Chromatographic column: silica gel chromatographic column (with a column length of 250mm and inside diameter of 4.6mm), or equivalent.
A.3.4.2 Mobile phase: n-hexane: n-amyl alcohol= 997:3.
A.3.4.3 Column temperature: 35℃.
1 Scope
2 Chemical name, structural formula, molecular formula and relative molecular mass
3 Technical requirements
Annex A Inspection method
Annex B Standard infrared spectrogram of vitamin D
Annex C High-performance liquid chromatography reference chromatogram of vitamin D3 and related substances
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
National food safety standard
Nutritional fortification substances in foods - Cholecalciferol (vitamin D3)
1 Scope
This standard is applicable to cholecalciferol (vitamin D3), a nutritional fortification substance in foods, which is prepared with lanolin cholesterol as raw material to obtain 7-dehydrocholesterol by chemical synthesis, ultraviolet irradiation and refining.
2 Chemical name, structural formula, molecular formula and relative molecular mass
2.1 Chemical name
(5Z,7E)-9,10-Secocholesta-5,7,10 (19)-triene-3β-ol
2.2 Structural formula
2.3 Molecular formula
C27H44O
2.4 Relative molecular mass
384.64 (according to the international relative atomic mass in 2018)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall meet those specified in Table 1.
Table 1 Sensory requirements
Item Requirement Inspection method
Color and luster Colorless or white Put a proper amount of sample into a clean and dry white porcelain dish, then observe its color and luster as well as state in natural light and smell it
Odor No odor or peculiar smell
State Acicular crystal or crystalline powder
3.2 Physical and chemical indexes
Physical and chemical indexes shall meet those specified in Table 2.
Table 2 Physical and chemical indexes
Item Index Inspection method
Content of vitamin D3, ω/% 97.0~103.0 A.3, Annex A
Specific rotation αm (20℃, D)/(°)·dm2·kg-1 +105.0~+112.0 A.4, Annex A
Absorption coefficient (265nm)
465~495 A.5, Annex A
Related substances: provitamin D3, trans-vitamin D3, tachysterol D3, 7-dehydrocholesterol Except for the peak of provitamin D3, the peak area of a single impurity shall not be greater than 0.5 times the main peak area of control solution; the sum of impurity peak areas shall not be greater than the main peak area of control solution A.6, Annex A
Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.75 or GB 5009.12
Total arsenic (by As)/(mg/kg) ≤ 2.0 GB 5009.76 or GB 5009.11
Note: Commercial products of cholecalciferol (vitamin D3) shall be made of cholecalciferol (vitamin D3) complying with this standard, and added with necessary food materials and/or food additives as auxiliary materials with the mass, range and consumption meeting the relevant requirements of corresponding national food safety standards.
Annex A
Inspection method
A.1 General requirements
Unless otherwise specified, analytically pure reagents or above and Class-III water specified in GB/T 6682 are adopted for the purposes of this standard. Unless otherwise specified, the standard solution used in the tests and the standard solution, preparations and products for determination of impurities are prepared in accordance with GB/T 601, GB/T 602 and GB/T 603. Unless otherwise specified, the solution used in the tests refers to the aqueous solution.
A.2 Identification test
A.2.1 Color reaction of acetic anhydride and concentrated sulfuric acid
A.2.1.1 Reagents and materials
A.2.1.1.1 Trichloromethane.
A.2.1.1.2 Acetic anhydride.
A.2.1.1.3 Sulfuric acid.
A.2.1.2 Identification method
Weigh 0.5mg sample, add 5mL trichloromethane to dissolve it, add 0.3mL acetic anhydride and 0.1mL sulfuric acid, shake it, it will turn yellow at first, gradually turn red, then turn purple and blue-green immediately, and finally turn green.
A.2.2 Infrared spectrum test
A.2.2.1 Reagents and materials
Potassium bromide.
A.2.2.2 Apparatus
Infrared spectrometer.
A.2.2.3 Analysis steps
Carry out test by potassium bromide pellet technique according to GB/T 6040, the infrared spectrum of the sample shall be consistent with the standard infrared spectrogram. See Figure B.1 for the standard infrared spectrogram of vitamin D3.
A.3 Determination of content of vitamin D3
A.3.1 Method summary
Determine vitamin D3 by high-performance liquid chromatography after dissolution and dilution, and calculate the content of vitamin D3 by external standard method.
A.3.2 Reagents and materials
A.3.2.1 n-hexane: chromatographically pure.
A.3.2.2 n-amyl alcohol: chromatographically pure.
A.3.2.3 Isooctane: chromatographically pure.
A.3.2.4 Vitamin D3 standard: with a mass fraction of not less than 98%.
A.3.2.5 7-dehydrocholesterol standard: with a mass fraction of not less than 98%.
A.3.2.6 Water: Class-I water complying with GB/T 6682.
A.3.3 Apparatus
High-performance liquid chromatograph: equipped with ultraviolet detector or equivalent detector.
A.3.4 Chromatography reference conditions
The recommended chromatographic column and typical chromatographic operating conditions are listed below; other chromatographic columns and chromatographic conditions which can reach the same separation may also be adopted.
A.3.4.1 Chromatographic column: silica gel chromatographic column (with a column length of 250mm and inside diameter of 4.6mm), or equivalent.
A.3.4.2 Mobile phase: n-hexane: n-amyl alcohol= 997:3.
A.3.4.3 Column temperature: 35℃.
Contents of GB 1903.50-2020
1 Scope
2 Chemical name, structural formula, molecular formula and relative molecular mass
3 Technical requirements
Annex A Inspection method
Annex B Standard infrared spectrogram of vitamin D
Annex C High-performance liquid chromatography reference chromatogram of vitamin D3 and related substances
