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Method for removing hyocholic acid from chenodeoxycholic acid

A technology of chenodeoxycholic acid and hyocholic acid, applied in the field of removing hyocholic acid, can solve the problems of poor effect, high cost, low efficiency, etc., achieve good separation effect and reduce volatilization

Active Publication Date: 2016-05-11
CHANGDE YUNGANG BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims at the above-mentioned problems of difficulty, poor effect, low efficiency and high cost in removing impurities of hyocholic acid, and provides a method for removing hyocholic acid from chenodeoxycholic acid that is simple, efficient, low-cost and has good removal effect. method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 120 kg of crude chenodeoxycholic acid extracted from pig bile (HPLC content 61.3%, see attached table 1 for specific detection indicators) that has been crudely separated and deoiled, put it into a 1000L enamel extraction kettle, add 600 kg of butyl acetate, Reflux for 1 hour after heating to boiling, add 12 kg of activated carbon, continue to stir and reflux for 1 hour, and then pass through a titanium rod filter unit for heat preservation and filtration to obtain a chenodeoxycholic acid butyl acetate solution.

[0014] Pump the chenodeoxycholic acid butyl acetate solution into a 1000L enamel precipitation kettle, cool to 40°C, add 12 kg of sec-butylamine, keep stirring for 1 hour, cool to room temperature 25°C, and crystallize for 4 hours to obtain a mixed suspension Cloudy liquid.

[0015] Put the mixed suspension into a D800 clean and sealed stainless steel centrifuge for centrifugation, and obtain chenodeoxycholic acid ammonium salt and butyl acetate mother li...

Embodiment 2

[0019] Take 110 kg of crude chenodeoxycholic acid extracted from pig bile (HPLC content 59.7%, see attached table 1 for specific detection indicators) that has been crudely separated and deoiled, and put it into a 1000L enamel extraction kettle, add 540 kg of butyl acetate, and heat Reflux for 1 hour after boiling, add 10 kg of activated carbon, continue to stir and reflux for 1 hour, and then pass through a titanium rod filter unit for heat preservation and filtration to obtain a chenodeoxycholic acid butyl acetate solution.

[0020] Pump the chenodeoxycholic acid butyl acetate solution into a 1000L enamel precipitation kettle, cool to 40°C, add 11 kg of sec-butylamine, keep stirring for 1 hour, cool to room temperature 25°C, and crystallize for 4 hours to obtain a mixed suspension Cloudy liquid.

[0021] The mixed suspension was put into a D800 clean and sealed stainless steel centrifuge, and centrifuged to obtain ammonium chenodeoxycholate and butyl acetate mother liquor, w...

Embodiment 3

[0025] Take 125 kg of crude chenodeoxycholic acid extracted from pig bile (HPLC content 63.3%, specific test indicators see attached table 1) that has been crudely separated and deoiled, and put it into a 1000L enamel extraction kettle, add 625 kg of butyl acetate, and heat Reflux for 1 hour after boiling, add 12.5 kg of activated carbon, continue to stir and reflux for 1 hour, then pass through a titanium rod filter unit for heat preservation and filtration to obtain a chenodeoxycholic acid butyl acetate solution.

[0026] Pump the chenodeoxycholic acid butyl acetate solution into a 1000L enamel precipitation kettle, cool to 40°C, add 12.5 kg of sec-butylamine, keep stirring for 1 hour, cool to room temperature 25°C, and crystallize for 4 hours to obtain a mixed suspension Cloudy liquid.

[0027] Put the mixed suspension into a D800 clean and sealed stainless steel centrifuge for centrifugation to obtain chenodeoxycholic acid ammonium salt and butyl acetate mother liquor, whe...

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PUM

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Abstract

The invention discloses a method for removing hyocholic acid from chenodeoxycholic acid. The method comprises the steps of dissolving, residue removing, complexing, crystallizing, centrifugal separating, emulsifying, acidifying, drying, mother liquor treating and the like; high-boiling-point butyl acetate is utilized as solvent, volatilization of the solvent is reduced, a good separation effect is achieved by utilizing the unique dissolution property of butyl acetate to impurities, and the solvent belongs to a three-level low-toxicity dangerous chemical; the selective complexing characteristic of sec-butylamine to bile acid is utilized, and the hyocholic acid and other impurities can be separated to a higher degree. According to the separation and purification method, impurity removing is qualified in one time, the loss rate of the chenodeoxycholic acid is 5% or below and is greatly lower than the effective ingredient loss of 30% in a conventional crystallization method, the solvent can be recycled, three wastes are not generated, and the method is an environment-friendly, low-cost and efficient separation method.

Description

technical field [0001] The invention relates to the technical field of chenodeoxycholic acid extraction, in particular to a method for removing hyocholic acid from chenodeoxycholic acid. Background technique [0002] Chenodeoxycholic acid is the main raw material for the synthesis of ursodeoxycholic acid. Due to the sharp increase in demand for ursodeoxycholic acid, the supply of chenodeoxycholic acid is in short supply. Pig bile is a biological non-renewable resource, its total bile acid content is 10%, and the chenodeoxycholic acid contained in it accounts for 40% of the total bile acid content, so it is a very excellent raw material for the production of chenodeoxycholic acid . However, since porcine bile also contains hyocholic acid, which accounts for 5% of the total bile acid content, and is similar in nature to chenodeoxycholic acid, it is easy to crystallize in the process of processing, extracting and purifying chenodeoxycholic acid. Separation method - selective ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 邓家国
Owner CHANGDE YUNGANG BIOTECHNOLOGY CO LTD
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