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Method for preparing chenodeoxycholic acid in pig bile by esterification method

A technique for chenodeoxycholic acid and hyodeoxycholic acid, which is applied in the field of preparing chenodeoxycholic acid in pig bile by an esterification method, can solve the problems of cumbersome steps, harsh reaction conditions, low product content and the like, and achieves a high extraction ratio , The preparation method is simple, and the effect of meeting the purity requirements

Inactive Publication Date: 2013-01-16
ANHUI KEBAO BIOLOGICAL ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the acquisition of CDCA is mainly based on cholic acid (CA) as a raw material and the method of extracting in bile (poultry bile and pig bile) is two major categories. 1. The steps are cumbersome and the reaction conditions require Harsh, not conducive to industrialized mass production; 2. When using the extraction method to obtain CDCA, it is mainly to use barium salt and calcium salt precipitation method, using barium salt to directly bring serious threats to the natural environment on which human beings live, and using calcium salt. A large amount of water is used, which is a great waste of water resources, and the content of the products obtained by the two extraction methods is low, generally less than 90%.
[0004] However, the current industrial production urgently needs a simple, safe and environmentally friendly method for extracting CDCA content greater than or equal to 98% chenodeoxycholic acid, but this method has not been reported at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The method for preparing chenodeoxycholic acid in porcine bile by esterification, the steps are as follows:

[0018] Small laboratory test, 1. Esterification: Take 0.1kg of the paste that has extracted bilirubin and hyodeoxycholic acid and put it into a laboratory vessel, add 3 times the amount of methanol and 4ml of concentrated sulfuric acid to dissolve it completely. After standing at room temperature for 10 hours, add sodium hydroxide to adjust the pH to 7.0, let it stand for 1 hour, filter with suction, put the filtrate in a rotary evaporator, set the vacuum degree of the rotary evaporator to 0.05Mpa, set the temperature to 45°C, and cool with circulating water Reclaim methanol to obtain esterification paste;

[0019] 2. Acylation: Take out the esterification paste obtained in step 1, put it into a container, add 1.0 times the amount of acetic anhydride, heat and stir to reflux for 1 hour, let it stand, put the liquid into the rotary evaporator, set the rotary evap...

Embodiment 2

[0028] During the pilot test, 1. Esterification: Take 10kg of the paste that has extracted bilirubin and hyodeoxycholic acid and put it into a test vessel, add 4 times the amount of methanol and 400ml of concentrated sulfuric acid to completely dissolve it, and leave it at room temperature and static After standing for 12 hours, add sodium hydroxide to adjust the pH to 6.5, let stand for 1-2 hours, filter with suction, put the filtrate in a rotary evaporator, set the vacuum degree of the rotary evaporator to 0.06Mpa, set the temperature to 45°C, and cool with circulating water Reclaim methanol to obtain esterification paste;

[0029] 2. Acylation: Take out the esterification paste obtained in step 1, put it into a container, add 1.3 times the amount of acetic anhydride, heat and stir to reflux for 2 hours, let it stand, put the liquid into the rotary evaporator, set the rotary evaporator The vacuum degree is 0.09Mpa, the set temperature is 95°C, and the circulating water is co...

Embodiment 3

[0038] In the production process, 1. Esterification: Take 100kg of the paste that has extracted bilirubin and hyodeoxycholic acid and put it into a container, add 5 times the amount of methanol and 4000ml of concentrated sulfuric acid to completely dissolve it, and let it stand at room temperature After 12 hours, add sodium hydroxide to adjust the pH to 6.0, let it stand for 2 hours, filter it with filter cloth, put the filtrate into the spherical concentrator, set the vacuum degree of the spherical concentrator to 0.07Mpa, set the temperature to 45°C, and recycle methanol by cooling with circulating water , to obtain esterified paste;

[0039] 2. Acylation: Take out the esterification paste obtained in step 1, put it into a container, add 1.5 times the amount of acetic anhydride, heat and stir to reflux for 3 hours, let it stand, put the liquid into the spherical concentrator, and set the spherical concentrator The vacuum degree is 0.1Mpa, the set temperature is 95°C, and the c...

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Abstract

The invention discloses a method for preparing chenodeoxycholic acid in pig bile by an esterification method, which comprises the following steps that: methanol, concentrated sulfuric acid and sodium hydroxide are used for esterification; acetic anhydride is used for acidylation; sherwood oil is used for extraction; the primary crystallization and the secondary crystallization are realized through ethanol and the sherwood oil; the sodium hydroxide is used for hydrolytic acidification; ethyl acetate and active carbon are used for crystallization; and the chenodeoxycholic acid is obtained through drying. The chenodeoxycholic acid is prepared by the method disclosed by the invention, the preparation method is simple, safety and environment protection are realized, the method can be used for large-scale industrial production, the content of the extracted chenodeoxycholic acid is higher or equal to 98 percent, the extraction rate is high, and the purity requirement on products in markets can be met.

Description

technical field [0001] The invention relates to a method for preparing chenodeoxycholic acid, in particular to a method for preparing chenodeoxycholic acid in pig bile by an esterification method. Background technique [0002] Chenodeoxycholic acid (CDCA for short) is an important biochemical substance present in animal bile, and is also one of the effective components of animal bile. It has pharmacological effects such as treating cholesterol-type stones, antibacterial, anti-inflammatory, anti-allergic, antipyretic, phlegm-reducing, and asthma-relieving. It is also the main raw material for the synthesis of expensive ursodeoxycholic acid. [0003] At present, the acquisition of CDCA is mainly based on cholic acid (CA) as a raw material and the method of extracting in bile (poultry bile and pig bile) is two major categories. 1. The steps are cumbersome and the reaction conditions require Harsh, not conducive to industrialized mass production; 2. When using the extraction me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
Inventor 郭庆徐宾朋张维秀赵厚发
Owner ANHUI KEBAO BIOLOGICAL ENG CO LTD
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