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Preparation method for high-purity solid dehydroascorbic acid

A technology for dehydroascorbic acid and ascorbic acid, which is applied in the directions of material separation, instruments, analytical materials, etc., to achieve the effects of easy control, high purity and simple process

Active Publication Date: 2009-11-04
石药集团维生药业(石家庄)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by the present invention is to overcome the shortcomings of the above-mentioned existing dehydroascorbic acid preparation methods, and provide a high-purity solid dehydroascorbic acid that does not need to use toxic substances in the preparation process, is safe, does not cause environmental pollution, and has a simple process. Preparation method of ascorbic acid

Method used

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  • Preparation method for high-purity solid dehydroascorbic acid
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  • Preparation method for high-purity solid dehydroascorbic acid

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Embodiment 1

[0030] A high-purity solid dehydroascorbic acid preparation method that does not need to use toxic substances in the preparation process, is safe, does not cause environmental pollution, and has a simple process, which is:

[0031] 1. Prepare the chromatography column

[0032] Take quantitative commercial silica gel, bake it at 110°C for 2 to 4 hours, then cool it to room temperature in a desiccator, wet-pack the column with acetonitrile, and set it aside;

[0033] 2. Oxidation of L-ascorbic acid (Vc)

[0034] In terms of weight ratio, weigh 237g of absolute ethanol, 10g of activated carbon, and 8g of L-ascorbic acid (Vc) according to the ratio of 29.625:1.25:1, add them to a three-necked bottle, stir at 20°C and feed in air, during which time sampling is used High-performance liquid chromatography is used for analysis to monitor the progress of the reaction. Ethanol volatilizes and is replenished in time until the end of the reaction;

[0035] 3. Remove activated carbon and...

Embodiment 2

[0040] A high-purity solid dehydroascorbic acid preparation method that does not need to use toxic substances in the preparation process, is safe, does not cause environmental pollution, and has a simple process, which is:

[0041] 1. Prepare the chromatography column

[0042] Take quantitative commercial silica gel, soak it in concentrated hydrochloric acid for 4 hours, filter it with suction, wash it with distilled water until it does not contain chloride ions, dry it and activate it in an oven at 120°C for 2 hours, then wet-pack it with acetonitrile for use;

[0043] 2. Oxidation of L-ascorbic acid (Vc)

[0044] In terms of weight ratio, weigh 316g of anhydrous methanol, 12g of activated carbon, and 8g of L-ascorbic acid (Vc) according to the ratio of 39.50:1.5:1, add them into a three-necked bottle, stir at 30°C and pass in air. High-performance liquid chromatography is used for analysis to monitor the progress of the reaction. Methanol volatilizes and replenishes in time...

Embodiment 3

[0050] A high-purity solid dehydroascorbic acid preparation method that does not need to use toxic substances in the preparation process, is safe, does not cause environmental pollution, and has a simple process, which is:

[0051] 1. Prepare the chromatography column

[0052] Take quantitative commercial silica gel, bake it at 100°C for 4 hours, then cool it to room temperature in a desiccator, and wet-pack the column with acetonitrile for use;

[0053] 2. Oxidation of L-ascorbic acid (Vc)

[0054] In terms of weight ratio, weigh 395g of absolute ethanol, 18g of activated carbon treated with 10% hydrochloric acid, and 10g of L-ascorbic acid (Vc) according to the ratio of 39.5:1.8:1, add them into a three-necked flask, stir at 40°C and pass in During the period, the air was continuously sampled and analyzed by high-performance liquid chromatography to monitor the progress of the reaction. Ethanol volatilized and replenished in time until the end of the reaction;

[0055] 3. ...

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Abstract

The invention relates to a preparation method for high-purity solid dehydroascorbic acid, which is obtained by the following steps: 1. oxidizing L-vitamin C (Vc); 2. removing active carbon and lower alcohol solvent; and 3. refining the dehydroascorbic acid. Compared with the previous method, the invention adopts the high efficiency liquid chromatography to analyze and monitor the process of oxidizing L-vitamin C so as to ensure the thorough reaction of the L-vitamin C, and adopts the column chromatography to refine the dehydroascorbic acid. The method has the advantages of simple process, easy control, safety without toxic substance and no environmental pollution. The analysis of the high efficiency liquid chromatography indicates that the content of dehydroascorbic acid in the solid prepared by the preparation method is up to more than 95% by using the area normalization method.

Description

technical field [0001] The invention relates to a method for preparing dehydroascorbic acid, in particular to a method for preparing high-purity solid dehydroascorbic acid that does not need to use toxic substances in the preparation process, is safe, does not cause environmental pollution, and has a simple process. Background technique [0002] Dehydroascorbic acid, also known as dehydroascorbic acid, English name: Dehydroascorbic acid, molecular formula: C 6 h 6 o 6 , the structural formula: [0003] [0004] Dehydroascorbic acid is a reversible oxidized form of ascorbic acid. It is active in nature and easily hydrolyzed to generate 2,3-diketoglutonic acid, which is further oxidized to threonic acid and oxalic acid and loses its physiological activity. [0005] [0006] In the presence of a hydrogen donor, dehydroascorbic acid can accept two hydrogen atoms and then convert into ascorbic acid, so it is difficult to purify. [0007] [0008] Dehydroascorbic acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62G01N30/02B01D15/08
Inventor 朱英刚王清格冯振英陈梦霞于春杰夏志华张宏霞范登科李会然
Owner 石药集团维生药业(石家庄)有限公司
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