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Preparation method of magnesium L-ascorbyl phosphate without any organic solvent residue

A technology of magnesium ascorbyl phosphate and organic solvents, applied in the field of biopharmaceuticals, can solve problems such as environmental pollution, affecting product quality, and difficulty in use, and achieve the effects of reducing production costs and improving dissolution rates

Inactive Publication Date: 2018-10-23
安徽顺利生物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adopt " phosphorus oxychloride " synthesis method to prepare L-ascorbyl magnesium phosphate, can cause serious pollution to environment, all do not advocate adopting at home and abroad; Adopt " phosphate " synthesis method to prepare L-ascorbyl magnesium phosphate, although this method It is a suitable method adopted by domestic manufacturers, but organic solvents are used to precipitate crystals during crystallization, and the residual organic solvents in the dried products cannot be removed; the residual organic solvents often make the products difficult to dissolve in water, and the products produced by some manufacturers are due to The residual amount of organic solvent exceeds the standard, and the dissolution lasts for more than tens of hours, which directly affects the product quality and causes great difficulties for the user

Method used

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  • Preparation method of magnesium L-ascorbyl phosphate without any organic solvent residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: Add oxalic acid to the L-ascorbyl phosphate crude product after the synthetic reaction according to the amount of VC input during the synthetic esterification reaction, take VC as 1 mass part, oxalic acid as 0.1-0.25 mass part, and decalcify , according to the concentration of crude L-ascorbyl phosphate, add deionized water in an appropriate amount, so that the concentration of the feed solution after decalcification of the organic acid is controlled at 1.0%, and the feed solution after decalcification is pumped into the ion resin exchange column at a speed of 0.1m Minutes, exchange and remove the cations;

[0017] The anion content of the treated feed liquid is measured to determine the amount of anion resin, and then it is treated with D008 macroporous strong base acrylic anion exchange resin to remove free phosphate and sulfate. This process needs to strictly determine the anion content to Determine the consumption of anion resin, guarantee the quality ...

example 2

[0022] Add oxalic acid to the crude product of L-ascorbyl phosphate after the synthesis reaction by the amount of VC input during the synthesis esterification reaction, take VC as 1 mass part, oxalic acid as 0.25-0.45 mass part, and carry out decalcification according to L - Add deionized water in an appropriate amount to the concentration of the crude product of ascorbyl phosphate, so that the concentration of the feed solution after decalcification of the organic acid is controlled at 15%. the cation;

[0023] The anion content of the treated feed liquid is measured to determine the amount of anion resin, and then it is treated with D008 macroporous strong base acrylic anion exchange resin to remove free phosphate and sulfate. This process needs to strictly determine the anion content to Determine the consumption of anion resin, guarantee the quality of L-magnesium ascorbyl phosphate feed solution before atomization drying crystallization.

[0024] After the fine filtration...

example 3

[0027] Example 3: drop into the consumption of VC during synthetic esterification reaction, add oxalic acid in the crude product of L-ascorbyl phosphate after synthetic reaction, take by weighing VC as 1 mass part, oxalic acid is 0.6-0.8 mass part, decalcify, Deionized water can be added in an appropriate amount according to the concentration of the crude L-ascorbyl phosphate, so that the concentration of the feed solution after decalcification of the organic acid is controlled at 20%. exchange to remove cations;

[0028] The anion content of the treated feed liquid is measured to determine the amount of anion resin, and then it is treated with D008 macroporous strong base acrylic anion exchange resin to remove free phosphate and sulfate. This process needs to strictly determine the anion content to Determine the consumption of anion resin, guarantee the quality of L-magnesium ascorbyl phosphate feed solution before atomization drying crystallization.

[0029] After the fine ...

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Abstract

The invention discloses a preparation method of magnesium L-ascorbyl phosphate without any organic solvent residue. The preparation method comprises following steps: (1) carrying out decationization;(2) removing cationic impurities; (3) removing anionic impurities; (4) carrying out atomization, drying, and crystallization; and (5) collecting materials, performing detection and packaging, and storing the products in a warehouse. The preparation method does not use any organic solvent, through direct atomization, drying, and crystallization, the production cost is reduced, the dissolution speedis increased, and magnesium L-ascorbyl phosphate does not have any organic solvent residue.

Description

technical field [0001] The invention relates to the field of biopharmaceuticals, in particular to a method for preparing magnesium L-ascorbyl phosphate without organic solvent residue. Background technique [0002] Two methods are mostly used in the market to prepare magnesium L-ascorbyl phosphate, one is the "phosphorus oxychloride" synthesis method to prepare magnesium L-ascorbyl phosphate, and the other is the "phosphate" synthesis method. Adopt " phosphorus oxychloride " synthetic method to prepare L-ascorbyl magnesium phosphate ester, can cause serious pollution to environment, all do not advocate adopting at home and abroad; Adopt " phosphate " synthetic method to prepare L-ascorbyl magnesium phosphate ester, although this method It is a suitable method adopted by domestic manufacturers, but organic solvents are used to precipitate crystals during crystallization, and the residual organic solvents in the dried products cannot be removed; the residual organic solvents o...

Claims

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Application Information

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IPC IPC(8): C07F9/655
CPCC07F9/65515
Inventor 李昊王虎杨春树张冬青
Owner 安徽顺利生物有限公司
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