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Method for producing ursodeoxycholic acid by using swine bladder as raw material

A technology of ursodeoxycholic acid and chenodeoxycholic acid, which is applied in the field of preparation of ursodeoxycholic acid, and can solve the problem of unnoticed removal of impurities such as fat and protein

Active Publication Date: 2008-07-09
苏州天绿生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] However, in all the above-mentioned pig bile acid preparation processes, NaOH is directly added to the original bile or the pig bile after extracting bilirubin for hydrolysis, and before the separation of chenodeoxycholic acid, ethyl acetate is used to separate pig bile. For oxycholic acid, no attention has been paid to the removal of impurities such as fat and protein in raw materials, the saving of solvents and the simplification of operation

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  • Method for producing ursodeoxycholic acid by using swine bladder as raw material
  • Method for producing ursodeoxycholic acid by using swine bladder as raw material
  • Method for producing ursodeoxycholic acid by using swine bladder as raw material

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Embodiment 1

[0031] Example 1: Separation of Precipitated Porcine Conjugated Bile Acid and Chenodeoxycholic Acid

[0032] Take fresh pig bile, add 3-4% saturated lime water, boil, generate bilirubin calcium salt precipitate, filter it out, and reserve it for the production of bilirubin for later use. Acidify the filtered bile with dilute hydrochloric acid to PH2-3, precipitate porcine conjugated bile acid, filter, boil and wash the filtered porcine conjugated bile acid with water twice, add about 8-10 times of 10% NaOH aqueous solution, heat and reflux for hydrolysis 20-24 hours, acidify with dilute hydrochloric acid or dilute sulfuric acid to PH8-9, heat to boil, after cooling, add 3-4% hydrogen peroxide to decolorize, then acidify with dilute hydrochloric acid to PH2-3, separate out free porcine bile acid, wash to medium sex. Add 15-20% NaOH aqueous solution and stir. At this time, hyodeoxycholic acid is difficult to dissolve and precipitate, and hyodeoxycholic acid and chenodeoxycholic...

Embodiment 2

[0034] Embodiment 2: the preparation of ursodeoxycholic acid

[0035] Take chenodeoxycholic acid 20g, dissolve in 1000ml glacial acetic acid, add sodium acetate 150-200g. After stirring to dissolve it, then add 15-20g of potassium chromate (in 100ml of water), let it stand at room temperature overnight, add 180-200ml of water, precipitate crystals, filter, wash with water, and dry to obtain a white powder, which is 3a-hydroxy- 7-ketocholanic acid (m.p.194-196°C), yield 84-85%.

[0036] Take 40g of 3a-hydroxy-7-ketocholanic acid and put it in a 3000ml three-neck bottle, add 1L of n-butanol and stir to dissolve, when the temperature rises to about 115-120°C, start adding 75-80g of sodium metal in portions. After reacting to the complete disappearance of the sodium metal on the liquid surface, white flocs are gradually separated out, continue to react for half an hour, add 1200ml of water and heat up under stirring to make it dissolve until transparent. Then the organic solvent...

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Abstract

The invention provides a process of separating anthrodsoxycholic acid by using fresh swine bile as raw material, the invention further provides a process for preparing ursodeoxycholic acid by using fresh swine bile as raw material, which comprises extracting conjugated bile acid from swine bile after acidification, removing foreign materials such as aliphatic acid and protein and the like, preparing purified pig bile acid through hydrolysis (saponification) and hydroperoxide decolourization, extracting anthrodsoxycholic acid through solution immersion cleaning, preparing ursodeoxycholic acid through oxidization and reduction of anthrodsoxycholic acid which is obtained through separating. The process of the invention improves the preparation technology of ursodeoxycholic acid, and achieves positive effects on the aspects of technology simplification and output increase.

Description

technical field [0001] The present invention relates to a preparation method of ursodeoxycholic acid, in particular to a preparation method of ursodeoxycholic acid using pig bile as a raw material. More specifically, the present invention provides a high-purity, high-yield A method for preparing ursodeoxycholic acid with high yield. Background technique [0002] Ursodeoxycholic acid (UDCA) for short is the main component of bear bile, and its chemical name is (3α, 7β)-dihydroxy-5βcholic acid, which is the 7β- Hydroxy epimers. Since the 1980s, when ursodeoxycholic acid was found to effectively dissolve cholesterol gallstones, new researches have shown that ursodeoxycholic acid has a positive effect on choleretic and liver protection. In recent years, it has been reported abroad that UDCA not only has a good effect on the treatment of primary biliary cirrhosis, primary sclerosing cholangitis, and chronic active hepatitis, but also can be used to treat chronic hepatitis and r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00A61K35/413A61P1/16
Inventor 陆其华张能荣
Owner 苏州天绿生物制药有限公司
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