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Method for extracting chenodeoxycholic acid from bile of fowl

A technique for chenodeoxycholic acid and bile acid, which is applied in the field of extracting chenodeoxycholic acid, can solve the problems of high toxicity of chemical substances, complicated process, low efficiency, etc., and achieves the advantages of convenient large-scale popularization and use, easy operation, and production equipment. The effect of high versatility

Inactive Publication Date: 2011-01-19
HUNAN CREDIT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reported extraction methods generally have the characteristics of complex process, high toxicity of chemical substances used, and environmental pollution, which makes chenodeoxycholic acid relatively low in efficiency under large-scale industrial production conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: get fresh or frozen chicken bile or other poultry bile, add industrial sodium hydroxide by 1 / 10 amount (W / V) of its volume, heat and boil 16 hours, after saponification is complete, cool to room temperature, add 1: 1 (V / V) hydrochloric acid to adjust pH2, precipitate crude bile acid; wash with water, dry in the shade.

[0023] Add crude bile acid to 10 times the amount of ethyl acetate, add saturated sodium chloride solution equal to the volume of ethyl acetate; dissolve, use 1% activated carbon by weight of crude bile acid; stir for 2 hours at 35°C, place, The carbon residue was filtered off, and the water layer was separated. Add an aqueous solution of nitrogen-containing organic compound A corresponding to 10% of the volume of the ester layer and a concentration of 20% into the ester layer. Stir at 60°C for 8 hours; cool, place, and separate the water layer; thin-layer chromatography analysis of the ester layer, most of the hydrophilic impurities such ...

Embodiment 2

[0026] Embodiment 2: get fresh or frozen chicken bile or other poultry bile, add industrial sodium hydroxide by 1 / 10 amount (W / V) of its volume, heat and boil about 16 hours, after saponification is complete, cool to room temperature; Add industrial calcium chloride to the solution according to 20% of the bile volume (W / V), react for 3 hours, filter, collect the precipitate, and dry.

[0027] Take crude bile acid calcium salt into 8 times the amount of water; adjust the pH to 2 with 1:1 (V / V) hydrochloric acid, add an equal volume of ethyl acetate, and separate the water layer; wash the ester layer with saturated sodium chloride solution to the middle After inactivation, add activated carbon equivalent to 1% of the weight of crude bile salt; stir for 1.5 hours at 45°C, let it stand, and filter off the carbon residue; Compound A in water. Stir at 65°C for 6 hours; cool, place, and separate the water layer; thin-layer chromatography analysis of the ester layer, 4 / 5 of the hydro...

Embodiment 3

[0030] Embodiment 3: get fresh or freezing chicken bile or other poultry bile, add industrial sodium hydroxide by 1 / 10 amount (W / V) of its volume, heat and boil about 16 hours, after saponification is complete, cool to room temperature, add 1 : 1 (V / V) hydrochloric acid to adjust pH2, precipitate crude bile acid; wash with water, dry in the shade.

[0031] Add crude bile acid to 12 times the amount of ethyl acetate, add saturated sodium chloride solution with 0.5 times the volume of ethyl acetate; dissolve; add diatomaceous earth equivalent to 3% of the weight of crude bile acid; 55 ° C, Stir for 3 hours, let it stand, separate the supernatant, let it stand, and separate the water layer. Add activated carbon equivalent to 0.5% of the weight of crude bile acid to the ester layer; stir at 50°C for 1 hour, let it stand, filter off the carbon residue, and separate the water layer. Add an aqueous solution of nitrogen-containing organic compound A corresponding to 15% of the volume...

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Abstract

A method for extracting chenodeoxycholic acid from bile of fowl comprises the following steps of: acquiring rough bile acid or rough bile acid calcium salt from fresh or frozen bile of fowl through saponification reaction, heating the bile acid resin solution together with the aqueous solution of organic nitrogenous compound A, removing the majority of hydrophilic impurities from the rough bile acid by using the organic nitrogenous compound A, reacting the acquired bile acid resin solution with organic nitrogenous compound B, dissolving the sediment, filtering, decolorizing and refining, so as to acquire chenodeoxycholic acid with a purity about 95%. The method of the invention has simple operation, the generality of the production equipment is high, and the chemic matter is harmless, therefore the invention is fit for industrialization of chenodeoxycholic acid.

Description

technical field [0001] The invention relates to a method for extracting bile acids, in particular to a method for extracting chenodeoxycholic acid (3α, 7α-dihydroxy-5β-cholic acid, CDCA for short) from poultry bile. Background technique [0002] Chenodeoxycholic acid has the effect of reducing the saturation of cholesterol in bile, so it has a good therapeutic effect on gallbladder stone disease. Chenodeoxycholic acid is also an important raw material for the chemical synthesis of ursodeoxycholic acid (3α, 7β-dihydroxy-5β-cholanic acid, referred to as: UDCA); ursodeoxycholic acid is the main active ingredient in bear bile , It has clear curative effect on various diseases such as liver and gallbladder. [0003] Extracting chenodeoxycholic acid from poultry bile is the main way of industrial production of chenodeoxycholic acid. The reported extraction methods generally have the characteristics of complex process, high toxicity of chemical substances used, and environmental ...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 刘小平彭伟易清风周智华米杰
Owner HUNAN CREDIT CHEM
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