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An optimized hyodeoxycholic acid crystallization process

A technology of hyodeoxycholic acid and process method, which is applied in the field of crystallization process to refine hyodeoxycholic acid, can solve the problems of prolonging the production cycle and limiting the source of crude products, and achieve the effects of inhibiting decomposition, wide source of raw materials, and low dosage

Active Publication Date: 2018-01-26
SHINEWAY PHARMA GRP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method not only needs to remove impurities in the early stage of the crude product, which prolongs the production cycle, but also requires the purity of the crude product to be not less than 70%, which limits the source of the crude product

Method used

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  • An optimized hyodeoxycholic acid crystallization process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 100g of magnesium hyodeoxycholic acid salt, the content is 55% based on hyodeoxycholic acid, add 450ml of ethyl acetate, and add 110ml of 50% dilute sulfuric acid solution, stir in a water bath at 60°C until there is no solid magnesium hyodeoxycholic acid Salt exists, discard the lower layer liquid, collect the upper layer liquid and filter, concentrate to 200ml, add 55ml 80% acetic acid solution, stir well, let stand for crystallization, filter to collect crystals, wash with appropriate amount of ethyl acetate, dry, pulverize, 31.64 g of hyodeoxycholic acid refined product was obtained, with a purity of 95%, a yield of 31.64%, and a transfer rate of 54.65%.

[0027] Wherein, yield=weight of refined hyodeoxycholic acid / weight of crude product of hyodeoxycholic acid×100%; transfer rate=(weight of refined product of hyodeoxycholic acid×content of refined product of hyodeoxycholic acid) / (weight of crude product of hyodeoxycholic acid×weight of hyodeoxycholic acid) Ox...

Embodiment 2

[0029] Weigh 200 g of the crude product of hyodeoxycholic acid (free acid), with a content of 73% based on hyodeoxycholic acid, add 1200 ml of ethyl acetate, and add 300 ml of dilute sulfuric acid, and stir in a water bath at 60 ° C until there is no solid hyodeoxycholic acid The crude product exists, discard the lower layer liquid, collect the upper layer liquid and filter, concentrate to 600ml, add 150ml 70% acetic acid solution, stir well, let stand for crystallization, filter to collect crystals, wash with appropriate amount of ethyl acetate, dry, pulverize, 124.23 g of hyodeoxycholic acid refined product was obtained, with a purity of 96%, a yield of 62.12%, and a transfer rate of 81.69%.

Embodiment 3

[0031] Weigh 200 g of hyodeoxycholic acid calcium salt, the content of which is 64% based on hyodeoxycholic acid, add 1000 ml of ethyl acetate, and add 260 ml of dilute sulfuric acid, and stir in a water bath at 70 ° C until no solid hyodeoxycholic acid calcium salt exists. Discard the liquid in the lower layer, collect the liquid in the upper layer and filter, concentrate to 500ml, add 130ml of 99% acetic acid solution, stir well, let stand to crystallize, collect the crystals by filtration, wash with an appropriate amount of ethyl acetate, dry, and pulverize to obtain hyodeoxygen Cholic acid refined product 95.41g, purity 96%, yield 47.70%, transfer rate 71.55%.

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Abstract

The invention relates to an optimized hyodeoxycholic acid crystallization process method. The process takes a crude produce with low content of hyodeoxycholic acid as a material, an ester solution is added to extract and concentrate, an organic acid is added, and the mixture stands and is subjected to crystallization and filtration to obtain a high-purity hyodeoxycholic acid. The organic acid is added in the recrystallization process to inhibit the dissolution of the ester solution, and reduce the acidity of a solution system, thereby being more favorable for the crystallization of the hyodeoxycholic acid which belongs to weak acid. Compared with a crystallization process with no addition of organic acid, the yield of the hyodeoxycholic acid is at least increased by more than 10%, and the transfer rate is at least increased by more than 15%.

Description

technical field [0001] The invention relates to a method for refining hyodeoxycholic acid by adopting a crystallization process, and belongs to the field of biomedicine. Background technique [0002] Hyodeoxycholic acid (3α, 6α-dihydroxycholic acid, HDCA) is extracted and processed from pig bile. It has the functions of lowering blood fat, antispasmodic, and expectorant. It is clinically used to treat hyperlipidemia and atherosclerosis. Sclerosis, tracheitis, viral upper respiratory tract inflammation in children, and indigestion caused by liver and gallbladder diseases; not only used to prepare artificial bezoar, but also an active ingredient in Qingkailing injection, which has been proved to have a significant effect on acute leukemia through clinical research Efficacy, in vitro experiments have proved that it can induce cell apoptosis and inhibit cell proliferation. [0003] At present, there are many methods for crystallizing hyodeoxycholic acid: Chinese Patent Publicat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 郝鹏彬杨琴冯玉康王文鹏孙胜斌姜国志
Owner SHINEWAY PHARMA GRP LTD
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