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Method for preparing hydroxycobalamin salt

A technology for obtaining hydroxocobalamin and methylcobalamin is applied in the field of preparing hydroxocobalamin, which can solve the problems of increased difficulty in extraction, low product purity, and high environmental protection investment, and achieves simple reaction product components, improved yield and purity, The effect of reducing the discharge of three wastes

Active Publication Date: 2014-04-02
HEBEI YUXING BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this technique is: because cyanocobalamin is a precursor, its property is stable, needs to add more than 4 kinds of chemical substances in the reaction and impels the reaction to complete, must strictly control temperature, PH in the reaction simultaneously, therefore, reaction is not easy to control, and The product is more complicated
At the same time, due to the excessive addition of chemical reagents, the generation of its residues or homologues increases the difficulty of subsequent extraction, and what is more serious is that the cyanide released from cyanocobalamin during the reaction needs to be completely removed in the reaction or subsequent extraction. , Occupational protection requirements are strict; in addition, there is a lack of layering process in the extraction process, and the function of macroporous resin is only used to concentrate the product, so the product purity is low
Simultaneously, the shortcoming of this technique also is owing to adding glacial acetic acid in the reaction and guarantees the pH of reaction, therefore has generated part hydroxocobalamin acetate during reaction, and in preparing hydroxocobalamin hydrochloride, hydroxocobalamin sulfate etc. When in the form of salt, it is necessary to add the corresponding acid to the crystallization stock solution for secondary conversion. Not only the process is long, but also because the conversion is not complete, hydroxocobalamin acetate becomes an impurity, and the subsequent impurity removal is only a crystallization one-step process, so , the product has high impurities. At present, the indicators stipulated by the European Pharmacopoeia are: content ≥ 96-102%, related substances ≤ 5%
In addition, since the crystallization adopts static crystallization, the crystallization time is long, more than 24h
The operation of the above process is difficult, the production cycle is long, the yield is low, the product impurities are high, the amount of waste produced is large, and the investment in environmental protection is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: the preparation of hydroxocobalamin acetate

[0028] Prepare 2.4Kg of methylcobalamin into a 2000 μg / ml methylcobalamin solution, adjust the pH to 3.18 with 20% acetic acid, turn on the air to stir, and illuminate under 17000LX until the content of hydroxocobalamin acetate in the reaction solution is 98.3% , the reaction solution is adsorbed on the styrene macroporous adsorption resin column, and the adsorption rate is 100L / h. After washing with water, it is developed with 450L acetone aqueous solution (wherein acetone: water=5:95), and the development rate is 100L / h. When the outlet color changes from light red to colorless, analyze 350L of 40% acetone aqueous solution through the resin column at a speed of 100-250L / h, collect the red crystal stock solution, start stirring, and add 600L to the crystal stock solution with a density of 0.810g / ml of acetone solution, stirred for 1h, allowed to stand for 4h, obtained hydroxocobalamin acetate 2.39Kg after suc...

Embodiment 2

[0029] Embodiment 2: the preparation of hydroxocobalamin hydrochloride

[0030] Prepare 2.4Kg of methylcobalamin into a 2000 μg / ml methylcobalamin solution, adjust the pH to 3.21 with 7% hydrochloric acid, turn on the air to stir, and illuminate under 17000LX until the content of hydroxocobalamin hydrochloride in the reaction solution is 98.4% , the reaction solution is adsorbed on the styrene macroporous adsorption resin column, and the adsorption rate is 100L / h. After washing with water, use 430L acetone aqueous solution (wherein acetone: water=6:94) to spread the layer, and the spread rate is 100L / h. When the outlet color changes from light red to colorless, pass 370L of 50% acetone aqueous solution through the resin column at a speed of 100-250L / h, collect the red crystal stock solution, start stirring, and add 600L to the crystal stock solution with a density of 0.810g / ml The acetone solution was stirred for 1 h, left to stand for 4 h, and 2.37 Kg of hydroxocobalamin hydr...

Embodiment 3

[0031] Embodiment 3: the preparation of hydroxocobalamin sulfate

[0032] 2.4Kg methylcobalamin was prepared into 2000 μg / ml methylcobalamin solution, adjusted pH to 3.20 with 20% sulfuric acid, turned on air stirring, irradiated under 17000LX until the content of hydroxocobalamin sulfate in the reaction solution was 98.2%, Adsorb the reaction solution on the styrene macroporous adsorption resin column, the adsorption rate is 100L / h, after washing with water, use 400L acetone aqueous solution (wherein acetone:water=5:95) to develop the layer, the rate of development is 100L / h, when the outlet When the color changes from light red to colorless, pass 340L of 40% acetone aqueous solution through the resin column at a speed of 100-250L / h, collect the red crystal stock solution, start stirring, and add 550L of crystal stock solution with a density of 0.810g / ml Acetone solution was stirred for 1 h, left standing for 4 h, and 2.36 Kg of hydroxocobalamin sulfate was obtained after suc...

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Abstract

The invention discloses a method for preparing hydroxycobalamin salt. The method comprises the following steps of: A, dissolving mecobalamin, and regulating the pH value to be 3.0 to 5.0 to obtain a liquid to be reacted; B, transforming the mecobalamin into the hydroxycobalamin salt with stirring through strong light irradiation so as to obtain a reaction liquid; C, absorbing the reaction liquid by using a macroporous resin, washing, developing by using a developing agent, and analyzing by using an analytical agent to obtain a crystallization stock solution; and D, adding acetone into the crystallization stock solution with stirring, dynamically crystallizing for 1 to 2h, standing for 4 to 5h, performing suction filtration, washing, and drying to obtain finished hydroxycobalamin salt. The method is easy to operate, high in stability and environment-friendly, the yield and the purity of products can be greatly improved, and the production cost is reduced at the same time.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing hydroxocobalamin salt. Background technique [0002] Hydroxocobalamin salts include hydroxocobalamin acetate, hydroxocobalamin hydrochloride, and hydroxocobalamin sulfate. They are vitamin B12 series products and are included in the European Pharmacopoeia. Because of their long retention time in the body, they are called For long-acting B12, it is an octahedral structure centered on cobalt ions. The molecular formula of hydroxocobalamin acetate is: C 64 h 93 CoN 13 o 17 P, the molecular weight is 1406; the molecular formula of hydroxocobalamin hydrochloride is: C 62 h 90 CLCoN 13 o 15 P, molecular weight: 1383, hydroxocobalamin sulfate C 124 h 180 co 2 N 26 o 34 P 2 S, molecular weight: 2791. Hydroxocobalamin salt is a dark red crystal or crystalline powder with strong hygroscopicity. It belongs to vitamin drugs and is used for the treatment a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H23/00C07H1/00C07C53/10C07C51/41
Inventor 张拴兵王玉锋
Owner HEBEI YUXING BIO ENG