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Purification method of hyodeoxycholic acid

A technology of hyodeoxycholic acid and its purification method, which is applied in the field of biochemical pharmacy, can solve the problems of ethyl acetate consumption, low product purity, and large reagent usage, and achieve the effect of simple operation method and overcoming low product purity

Active Publication Date: 2012-08-01
JIANGSU QINGJIANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In method 2, hyodeoxycholic acid is very slightly soluble in ethyl acetate, and this method needs to consume a large amount of ethyl acetate; in method 1 and method 2, the reagent usage is large, and the product purity is low; the hyodeoxycholic acid obtained in method 3 The acid content can still only reach >98.5%, and the carcinogen benzene is used in the process

Method used

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  • Purification method of hyodeoxycholic acid
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  • Purification method of hyodeoxycholic acid

Examples

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Effect test

Embodiment 1

[0021] Take 10g of crude hyodeoxycholic acid and add it to a beaker, then add 3000ml of ammonia water with a mass concentration of 1.0%, the content of hyodeoxycholic acid in the solution is 3.3%, keep the temperature to room temperature, stir for 5min, filter to remove insoluble impurities, collect the filtrate, and the yield More than 99%; add 500ml ethyl acetate to the collected filtrate, stir thoroughly for 5 minutes, let it stand for 6 hours, remove ethyl acetate by siphon, and obtain the aqueous phase liquid, the yield is 97%; put the aqueous phase liquid in a beaker, slowly drop Add hydrochloric acid solution with a mass concentration of 10.0%, adjust the pH value to 7.2 with a pH meter, continue to stir slowly for 1 min, cool to 0°C, let stand for 6 h to crystallize, filter, wash the filter cake with 1000 ml of purified water, and dry under reduced pressure 9.1 g of white crystalline hyodeoxycholic acid was obtained, with a yield of 90%. The melting point is above 197....

Embodiment 2

[0023] Take 10g of crude hyodeoxycholic acid and add it to a beaker, then add 2750ml of ammonia water with a mass concentration of 1.0%, the content of hyodeoxycholic acid in the solution is 3.6%, keep the temperature to room temperature, stir for 5min, filter to remove insoluble impurities, collect the filtrate, and the yield More than 98%; add 450ml ethyl acetate to the collected filtrate, stir thoroughly for 5 minutes, let it stand for 6 hours, remove ethyl acetate by siphon, and obtain the aqueous phase liquid, the yield is 96%; put the aqueous phase liquid in a beaker, slowly drop Add hydrochloric acid solution with a mass concentration of 10.0%, adjust the pH value to 7.1 with a pH meter, continue to stir slowly for 1 min, cool to 0°C, let stand for 6 h to crystallize, filter, wash the filter cake with 900 ml of purified water, and dry under reduced pressure 8.8 g of white crystalline hyodeoxycholic acid was obtained, with a yield of 89%. The melting point is above 197.5...

Embodiment 3

[0025] Take 10g of crude hyodeoxycholic acid and add it to a beaker, then add 2500ml of ammonia water with a mass concentration of 1.0%, the content of hyodeoxycholic acid in the solution is 4.0%, keep the temperature to room temperature, stir for 5min, filter to remove insoluble impurities, collect the filtrate, and the yield More than 97%; add 600ml ethyl acetate to the collected filtrate, stir thoroughly for 5 minutes, let it stand for 6 hours, remove ethyl acetate by siphon, and obtain the aqueous phase liquid, the yield is 98%; put the aqueous phase liquid in a beaker, slowly drop Add a hydrochloric acid solution with a mass concentration of 10.0%, adjust the pH value to 7.0 with a pH meter, continue stirring slowly for 1 min, cool to 0°C, let stand for 6 h to crystallize, filter, wash the filter cake with 800 ml of purified water, and dry under reduced pressure 9.0 g of white crystalline hyodeoxycholic acid was obtained, with a yield of 91%. The melting point is above 19...

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Abstract

The invention discloses a purification method of a hyodeoxycholic acid. The purification method of the hyodeoxycholic acid comprises the following steps that: a hyodeoxycholic acid crude product is dissolved with aqueous ammonia to remove insoluble impurities by filtration, and a filtrate is collected; in the collected filtrate, ethyl acetate is added and allowed to keep stand to remove a fat-soluble substance, and the ethyl acetate is removed by siphoning to obtain an aqueous phase liquid; and in the aqueous phase liquid, a hydrochloric acid solution is added dropwise to adjust the pH value, and then crystallization, filtration, water wash and drying are carried out to obtain a hyodeoxycholic acid pure product. According to the purification method provided by the invention, the process route is direct, the operation is simple, the environment is protected, the purity of the obtained product HPLC (High-Performance Liquid Chromatography) is more than or equal to 99.8%, and the defects that the purity of a product obtained by the traditional method is not high, and a toxic carcinogen benzene needs to be used are overcome.

Description

technical field [0001] The invention relates to a purification method in the field of biochemical pharmacy, in particular to a purification method of hyodeoxycholic acid. technical background [0002] The content of hyodeoxycholic acid in pig bile is 8.5~12%. Hyodeoxycholic acid is a blood lipid-lowering drug, which can inhibit the formation of cholic acid and dissolve fat, reduce blood cholesterol and triglyceride, and is suitable for type Ia or type Ib hyperlipidemia and atherosclerosis. It has a certain antibacterial effect on pertussis bacillus, diphtheria bacillus, and staphylococcus aureus, and can be used as an anti-inflammatory drug to treat chronic bronchitis and viral upper respiratory tract inflammation in children. This product can stimulate the secretion of bile and make the bile thinner without increasing the amount of solids. It is suitable for cholangitis, cholecystitis, cholelithiasis and other non-obstructive cholestasis; it can also accelerate the gallbla...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 王崇益陈文静
Owner JIANGSU QINGJIANG PHARMA
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