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Process for preparing hyodeoxycholic acid

A hyodeoxycholic acid and process technology, applied in the directions of steroids, organic chemistry, etc., can solve the problems of high cost, low recovery rate, high solvent toxicity, etc., and achieve the effects of low cost, easy operation and simple operation

Active Publication Date: 2012-11-14
NANJING XINBAI PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the product obtained by other extraction and purification processes has problems such as low purity, high solvent toxicity, low recovery rate, and high cost, which requires a new method to solve these problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Salting out: Use 50.0g of leftovers from bilirubin extraction as raw materials, add them to the reaction kettle, add 225mL of water to prepare a solution, adjust the pH to 3.0 with HCl solution, and control the temperature at about 20°C while stirring While adding 79g NaCl, when the salt is completely dissolved, continue to stir for 45min, and filter with suction to obtain a filter cake;

[0028] (2) Alkaline hydrolysis: Take out the filter cake in step (1), weigh it to 35.4g, put it into the reaction kettle, then add 90mL of 0.4g / mL KOH solution for hydrolysis, hydrolyze for 45min, and acidify with HCl solution to Congo red turns blue, precipitates out and stands still for 1.5h, then filters with suction to obtain a filter cake;

[0029] (3) Adsorption decolorization: Take out the filter cake in step (2), weigh 18.6g, put it into the reaction kettle, add 74mL ethyl acetate and 1.5g medical activated carbon, heat to 77°C, condense and reflux for 45min, cool to Suct...

Embodiment 2

[0036] (1) Salting out: Use 50.0g of leftovers from bilirubin extraction as raw materials, add them to the reaction kettle, add 300mL of water to prepare a solution, and use H 2 SO 4 Adjust the pH of the solution to 4.0, control the temperature at about 25°C, add 120g NaCl while stirring, continue stirring for 60 minutes after the salt is completely dissolved, and filter with suction to obtain a filter cake;

[0037] (2) Alkaline hydrolysis: Take out the filter cake in step (1), weigh 36.2g, add it to the reaction kettle, add 0.4g / mL NaOH solution 108mL, hydrolyze for 60min, and use H 2 SO 4 The solution was acidified until the Congo red turned blue, precipitated and allowed to stand for 2 hours, then filtered with suction to obtain a filter cake;

[0038] (3) Adsorption decolorization: Take out the filter cake in step (2), weigh 17.7g, put it into the reaction kettle, add 88mL acetone and 1.5g medical activated carbon, heat to 80°C, condense and reflux for 60min, and cool t...

Embodiment 3

[0045] (1) Salting out: Add 100.0g of leftovers from bilirubin extraction as raw materials to the reaction kettle, add 300mL of water to prepare a solution, adjust the pH to 2.0 with HCl solution, and control the temperature at about 15°C while stirring While adding 90g NaCl, when the salt is completely dissolved, continue to stir for 30 minutes, and filter with suction to obtain a filter cake;

[0046] (2) Alkaline hydrolysis: Take out the filter cake in step (1), weigh 72.5g, add it to the reaction kettle, add 145mL of 0.35g / mL KOH solution, hydrolyze for 30min, acidify with HCl solution until Congo red Blue, after precipitation, let it stand for 1h, filter with suction, and obtain a filter cake;

[0047] (3) Adsorption decolorization: Take out the filter cake in step (2), weigh 37.2g, add it to the reaction kettle, add 112mL acetone and 2.3g medical activated carbon, heat to 65°C, condense and reflux for 30min, and cool to 20°C , suction filtration, adding 23g of anhydrous...

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PUM

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Abstract

The invention discloses a process for preparing hyodeoxycholic acid and belongs to the field of biological pharmacy. The extraction and purification process comprises the following steps of: leftover salting-out, alkaline hydrolysis, dissolution and discoloring, filtering and dewatering, concentrated crystallization and vacuum-drying to obtain a crude product; and methyl esterification, column chromatography separation, alkaline hydrolysis again, purification, finished product vacuum-drying and the like. The process has the advantages that an obtained product has high purity, is free from extraneous odor and is environmentally friendly, a solvent can be recycled, and the process is easy to operate, has low cost, is simple and safe to operate and can be used for industrial production.

Description

technical field [0001] The invention relates to a process for preparing hyodeoxycholic acid, specifically a new process for preparing medical hyodeoxycholic acid from leftovers (or pig bile) for extracting bilirubin by using the principles of salting out, methyl esterification and recrystallization, It belongs to the field of biopharmaceuticals. technical background [0002] Hyodeoxycholic Acid (HDCA) is a biochemical substance widely present in animal bile, the content is 0.1%~0.2%, and the molecular formula is C 24 h 40 o 4 , the molecular weight is 392.58. It is slightly soluble in alcohol, slightly soluble in acetone, very slightly soluble in ether and chloroform, and almost insoluble in water. my country is rich in pig gall resources. Pig bile mainly contains bile acids, bile pigments, mucin, lipids and inorganic substances, etc., and bile acids mainly include hyodeoxycholic acid, hyodeoxycholic acid, chenodeoxycholic acid, 3α- Hydroxy-6-oxo-5α-cholanic acid and gal...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 沈飞胡永红于辉李栋芸曹峥冯旌杨文革
Owner NANJING XINBAI PHARMA
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