Non-organic solvent extraction method for chenodeoxycholic acid in bird gall

A chenodeoxycholic acid, non-organic technology, applied in the field of extraction of chenodeoxycholic acid, can solve the problems of complex extraction process, environmental pollution and high production cost

Inactive Publication Date: 2008-03-19
刘永存
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past, the production processes of chenodeoxycholic acid mainly include barium chloride salt method, calcium chloride salt method, etc. No matter which method is used, organic solvents must be used in the extra...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Embodiment 1: take poultry gall, chop, filter, add 5% sodium hydroxide of bile mass, stir and dissolve, heat and boil to carry out saponification reaction, time 20 hours; Saponification solution adds 10% hydrochloric acid solution to neutralize and adjust pH to 2 , stir, stand still, filter, and collect the precipitated total bile acids; add 5% sodium hydroxide solution to dissolve the total bile acids, add 10% of its mass of activated carbon, heat and reflux for 1 hour for decolorization, and add 10% of mass of chlorinated bile acids to the filtrate Calcium, keep stirring, stand still, collect the precipitate; add 10% sodium carbonate to the calcium salt precipitate, heat and reflux for 1 hour to decalcify; filter, adjust the pH2 of the filtrate with 5% hydrochloric acid solution, stand still, filter, collect the precipitate, and vacuum dry , the crude product of chenodeoxycholic acid was obtained with a purity of 52% (HPLC).

Embodiment 2

[0008] Example 2: Take poultry bile, add 5% of its mass of sodium hydroxide, stir to dissolve, heat and boil for saponification reaction for 22 hours; add 10% hydrochloric acid to the saponification solution to neutralize and adjust pH to 3, stir, and let stand , filtered, and the precipitate was collected to obtain the total bile acid; the total bile acid was dissolved in 5% sodium hydroxide solution, and then 10% of its mass of activated carbon was added, heated to reflux for decolorization for 1 hour, and the filtrate was added with 12% of its mass of calcium chloride, continuously Stir, stand still, and collect the precipitate; add 10% sodium carbonate to the calcium salt precipitate, heat and reflux for 2 hours, decalcify, filter, adjust the pH3 of the filtrate with 7% hydrochloric acid solution, let stand, filter, collect the precipitate, and vacuum dry to obtain Chenodeoxycholic acid crude product, purity 52.8% (HPLC).

Embodiment 3

[0009] Embodiment 3: Take poultry bile, add its mass 5% sodium hydroxide, stir to dissolve, heat and boil for saponification reaction, time is 24 hours; saponification solution is added with 10% hydrochloric acid solution to neutralize and adjust Ph4, stir, stand still, filter , collect the precipitate to get the total bile acid; add 5% sodium hydroxide solution to dissolve the total bile acid, then add 10% of its mass of activated carbon, heat and reflux for decolorization for 1 hour, add 14% of its mass of calcium chloride to the filtrate, and keep stirring. Stand still and collect the precipitate; add 15% sodium carbonate to the calcium salt precipitate, heat and reflux for 3 hours, and decalcify; filter, and adjust the pH of the filtrate to 3.5 with 10% hydrochloric acid solution, let stand, filter, collect the precipitate, and dry in vacuum to obtain goose Deoxycholic acid crude product, purity 56.89% (HPLC).

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PUM

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Abstract

The present invention discloses an extraction method of the inorganic solvent of chenodeoxycholic acid in the avian bile. The first step is a saponification reaction, that is, the avian bile and sodium hydroxide are boiled and saponified according to a certain proportion, and the saponification lasts twenty to twenty four hours; the second step is a counteraction reaction, that is, saponification solution is counteracted by hydrochloric acid, the pH value is regulated to two to four, and after deposition, total bile acid is generated; the third step is the calcium salt deposition, that is, the total bile acid is resolved in oxyhydrogen sodium solution, and after the addition of activated carbon, refluence and filtration, the calcium salt deposit is obtained by adding ten to fourteen percent of calcium chloride into filtrate; the fourth step is decalcification, that is, sodium carbonate is added into calcium salt according to a proportion between ten percent and fifteen percent, heating and refluence last one to three hours, and the pH value of filtrate is regulated to 2.0 to 3.5 by five to ten percent of hydrochloric solution, so that deposit is obtained; the fifth step is the collection of the deposit, that is, the crude chenodeoxycholic acid is generated by vacuum drying. Ethanol and 120 # gasoline are not needed, the investment of equipment is reduced, the process cycle is shortened, and the cost of extraction is reduced.

Description

Technical field [0001] The invention relates to a method for extracting chenodeoxycholic acid, in particular to a method for extracting chenodeoxycholic acid with a non-organic solvent. Background technique [0002] Chenodeoxycholic acid (CDCA for short) is a natural product extracted from poultry bile. In the past, the production processes of chenodeoxycholic acid mainly include barium chloride salt method, calcium chloride salt method, etc. No matter which method is used, organic solvents must be used in the extraction process: such as ethanol, 120# gasoline, etc. , so that the extraction process is complicated and easy to cause environmental pollution, and the production cost is correspondingly high due to the long production cycle. Contents of the invention [0003] The purpose of the present invention is to provide a non-organic solvent extraction method for chenodeoxycholic acid in poultry bile, extract and prepare chenodeoxycholic acid in alkalized and acidified aq...

Claims

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Application Information

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IPC IPC(8): C07J9/00A61K35/413A61K35/57
Inventor 李良铸刘永存张晓雯
Owner 刘永存
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