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Hyodeoxycholic acid refining method

A technique for refining hyodeoxycholic acid, which is applied in the field of high-purity hyodeoxycholic acid and the refining of hyodeoxycholic acid, can solve the problems of reduced product yield, long production cycle, unfavorable large-scale production, etc., and achieve product quality High, low production cost, high production efficiency

Active Publication Date: 2013-06-19
SHINEWAY PHARMA GRP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the solubility of methanol, ethanol, ethylene glycol, isopropanol, and N,N-dimethylformamide to HDCA is too high, water is added to reduce the solubility for crystallization, which is a very conventional crystallization method, and Due to the nature of this product, no crystals are precipitated after adding water, but only cloudy, and then filtered, which is not conducive to large-scale production
In addition, if the recrystallization process is used, the yield of the product will be greatly reduced
[0006] In summary, in order to improve the safety and compliance of HDCA medication, and overcome the defects of the existing HDCA purification methods such as product smell, cumbersome process, difficult operation, long production cycle, and high cost, it is urgent to develop a method that is easy to process large-scale production, Refining method for preparing odorless high-purity HDCA with advantages of low cost and short production cycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 750g of crude hyodeoxycholic acid (melting point 172.5°C-174.7°C, purity 72%), add ethyl acetate for reflux extraction 3 times, each time add 3000ml of ethyl acetate, reflux extraction for 30 minutes, filter, discard the filtrate, Add ethyl acetate to the dregs and extract 12 times under reflux, each time add 3000ml of ethyl acetate, reflux extract for 30 minutes, let cool, filter, when the filtrate is concentrated until hot, when crystals are precipitated, filter, dry and crush the residue to obtain white pig gourd. Oxycholic acid finished product 393g, yield 52.4%. The melting point is 196.9°C to 197.7°C.

[0025] The hyodeoxycholic acid (HDCA) content in the finished product is 99.4%. No fishy smell.

Embodiment 2

[0027] Take 750g of the crude product of hyodeoxycholic acid (melting point is 172.5℃~174.7℃), add ethyl acetate for reflux extraction 4 times, each time add 2250ml of ethyl acetate, reflux extraction for 30 minutes, filter, discard the filtrate, add acetic acid to the dregs Ethyl extraction was carried out 18 times, each time adding 2250ml of ethyl acetate, reflux extraction for 30 minutes, filtering, the filtrate was concentrated until hot, and when crystals were precipitated, let it cool, filtered, and the residue was dried and pulverized to obtain 386g of white hyodeoxycholic acid product. The yield is 51.5%, the melting point is 197.5°C-198.1°C, the HDCA content is 98.9%, and there is no fishy smell.

Embodiment 3

[0029] Take 750g of crude hyodeoxycholic acid (melting point: 172.5℃~174.7℃), add propyl acetate to reflux for extraction 4 times, each time add 3500ml of propyl acetate, reflux and extract for 30 minutes, filter, discard the filtrate, add propyl acetate to the dregs Esters were refluxed for 20 times, each time adding 3500ml of propyl acetate, refluxed for 25 minutes, filtered, the filtrate was concentrated until hot, and when crystals were precipitated, let it cool, filtered, and the residue was dried and crushed to obtain 380g of white hyodeoxycholic acid product. The yield is 50.7%, the melting point is 196.7°C-198.2°C, the HDCA content is 98.4%, and there is no fishy smell.

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Abstract

The invention relates to a hyodeoxycholic acid refining method. The hyodeoxycholic acid refining method comprises the following steps of carrying out reflux extraction of a hyodeoxycholic acid crude product having a melting point above 170 DEG C 9 to 45 times by an ester organic solvent, rejecting the extract obtained by the 1 to 5th reflux extraction processes, collecting the extract obtained by the 6 to 45th reflux extraction processes, carrying out concentration heating until crystals are precipitated, cooling, carrying out filtration, and drying and crushing the filter residues to obtain hyodeoxycholic acid having high purity greater than 98%, a melting point greater than or equal to 196.5 DEG C, a melting range less than 2 DEG C and no fishy smell. The hyodeoxycholic acid refining method has the advantages of high product quality, high yield, high production efficiency, low production cost, simple processes and good repeatability, is suitable for pharmacy industrial application and has a good application prospect.

Description

technical field [0001] The invention relates to a method for refining hyodeoxycholic acid, in particular to a method for preparing hyodeoxycholic acid with no fishy smell and high purity from crude hyodeoxycholic acid with a melting point above 170°C, belonging to the field of biomedicine . Background technique [0002] Hyodeoxycholic acid (Chenodeoxycholic Acid, HDCA) is a biochemical substance widely present in animal bile, with a content of 0.1% to 0.2%. Its chemical name is 3α,6α-dihydroxy-5β-cholanic acid, and its molecular formula is C24H40O4. The molecular weight is 392.58, easily soluble in ethanol, slightly soluble in acetone, very slightly soluble in ethyl acetate, chloroform or ether, almost insoluble in water. HDCA has the effects of lowering blood fat, antispasmodic and expectorant, and is clinically used to treat hyperlipidemia, atherosclerosis, tracheitis, viral upper respiratory tract inflammation in children, and dyspepsia caused by liver and gallbladder di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 赵伯友陈浩达冯玉康姜国志孙胜斌张岩岩
Owner SHINEWAY PHARMA GRP LTD
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