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Method for extracting chenodeoxycholic acid from pig gall paste

A technology of chenodeoxycholic acid and pig gall paste, which is applied in the fields of steroids and organic chemistry, can solve the problems of low extraction yield, difficult separation, waste of water resources, etc., and achieve improved extraction yield and good separation effect Effect

Active Publication Date: 2020-02-14
HUNAN JIUDIAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] From the structural comparison, it can be seen that the structural difference between hyodeoxycholic acid (HDCA) and the target extract chenodeoxycholic acid (CDCA) is only a difference in the position of hydroxyl substitution, while hyodeoxycholic acid (HCA) is different than chenodeoxycholic acid. (CDCA) has one more hydroxyl group, and the similarity in structure makes it difficult to separate the three substances
[0011] The existing extraction methods are mainly barium salt method and calcium salt precipitation method, crystallization extraction method, ion exchange resin method, barium salt will bring serious environmental problems, and when calcium salt is used, a very large amount of water will be used, which is a great waste Water resources are exhausted, the crystallization extraction method needs to use a large amount of organic solvent, the mother liquor needs to be separated and crystallized repeatedly, the production cycle is long, and it cannot be produced on a large scale. The extraction yield of these methods is low, and the purity of the product obtained is generally lower than 90%. It can separate several components in pig bile at one time

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  • Method for extracting chenodeoxycholic acid from pig gall paste
  • Method for extracting chenodeoxycholic acid from pig gall paste
  • Method for extracting chenodeoxycholic acid from pig gall paste

Examples

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Effect test

Embodiment 1

[0060] A method for extracting chenodeoxycholic acid from pig bile paste, which is an embodiment of a laboratory test, has included the following steps:

[0061] (1) Saponification: take 3 kg of pig gall paste (HPLC content 22.1%), the pig gall paste is dark brown and is a blocky solid. Put it into a 30L reaction kettle, add 9 kg of water and 1.2 kg of sodium hydroxide, heat to reflux at 100°C for saponification, and the duration of saponification is 12 hours.

[0062] (2) Complexation crystallization: reflux the saponified reaction solution for 8 hours and cool it to 48°C, add hydrochloric acid to adjust the pH to 10, then add magnesium chloride aqueous solution (1.5 kg magnesium chloride hexahydrate dissolved in 3.3 kg water), and stir at 50°C After 4 hours, filter and rinse with 0.6 kg of water to obtain filtrate and filter cake. The filter cake is hyodeoxycholic acid magnesium salt, and the filtered hyodeoxycholic acid magnesium salt is added with water and acid to dissoc...

Embodiment 2

[0082] A method for extracting chenodeoxycholic acid from pig bile paste, which is the second embodiment of the laboratory test, has included the following steps:

[0083] (1) Saponification: take 3 kg of pig gall paste (HPLC content 22.1%), the pig gall paste is dark brown and is a blocky solid. Put it into a 30L reaction kettle, add 9 kg of water and 1.2 kg of sodium hydroxide, heat to reflux at 100°C for saponification, and the duration of saponification is 12 hours.

[0084] (2) Complexation and crystallization: reflux the saponified reaction solution for 8 hours and cool it to 40°C, add hydrochloric acid to adjust the pH to 11, then add magnesium chloride aqueous solution (1.8 kg of magnesium sulfate heptahydrate dissolved in 3.3 kg of water), 35°C Stir for 4 hours, then filter and rinse with 0.6 kg of water to obtain filtrate and filter cake. The filter cake is hyodeoxycholic acid magnesium salt, and the filtered hyodeoxycholic acid magnesium salt is added with water an...

Embodiment 3

[0096] A method for extracting chenodeoxycholic acid from pig bile paste, which is an embodiment of a pilot test in a factory, has included the following steps:

[0097] (1) Saponification: take 90 kg of pig gall paste (HPLC content 22.1%), the pig gall paste is dark brown and is a blocky solid. Put it into a 1000L reactor, add 270 kg of water and 36 kg of sodium hydroxide, heat to reflux at 98°C for saponification, and the duration of saponification is 12 hours.

[0098] (2) Complexation and crystallization: reflux the saponified reaction solution for 8 hours and cool it to 44°C, add hydrochloric acid to adjust the pH to 9, then add magnesium chloride aqueous solution (45 kg magnesium chloride hexahydrate dissolved in 100 kg water), at 42°C Stir for 4 hours, then filter and rinse with 18 kg of water to obtain filtrate and filter cake. The filter cake is hyodeoxycholic acid magnesium salt, and the filtered hyodeoxycholic acid magnesium salt is added with water and acid to dis...

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Abstract

The invention discloses a method for extracting chenodeoxycholic acid from pig gall paste. The method comprises the steps such as saponification, complexation crystallization, extraction esterification and acetylation, and the purpose that hyodeoxycholic acid, hyocholic acid and the chenodeoxycholic acid are separate from the pig gall paste in one time is achieved. The purity of the obtained threetypes of products is high, reagents are all cheap and easy to obtain, most solvents can be recycled and reused, and produced waste water is less.

Description

technical field [0001] The invention belongs to the field of separation and purification, in particular to a method for extracting chenodeoxycholic acid from pig gall paste. Background technique [0002] Chenodeoxycholic acid (chenodeoxycholic acid, CDCA), the chemical name is 3α,7α-dihydroxy-5β-cholanic acid, CAS number: 474-25-9, the molecular formula is C24H40O4, the molecular weight is 392.57, and the structural formula is as follows: [0003] . [0004] Chenodeoxycholic acid is a substance mainly extracted from bile. It is mainly used to reduce the saturation of cholesterol in bile. It is mainly used in the treatment of gallstones clinically. The main raw material of UDCA), in 1972, the treatment of dissolving cholesterol gallstones was officially developed by the United Kingdom, and chenodeoxycholic acid was used as the first drug to correct saturated bile and dissolve gallstones. It is now known that chenodeoxycholic acid is contained in the bile, liver, kidney an...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 廖泽斌王湘武宁虎林肖稳定郑霞辉
Owner HUNAN JIUDIAN PHARMA
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