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Method for preparing chenodeoxycholic acid by extraction complexing process

A technology of chenodeoxycholic acid and complexation, applied in the field of preparation of chenodeoxycholic acid by extraction and complexation, can solve the problems of less organic solvent consumption, less environmental pollution, benzene/toluene environmental pollution, etc. Big, little effect

Pending Publication Date: 2020-12-01
ANHUI KEBAO BIOLOGICAL ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to solve the problem of environmental pollution of benzene / toluene used in the extraction process of chenodeoxycholic acid in pig bile and the waste of water resources by calcium salt method in view of the deficiencies of the above technologies, and to provide an extraction and complexation method Separation and purification of chenodeoxycholic acid from pig bile, this method has the characteristics of high yield, high purity, less organic solvent consumption, and less environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Extraction: Add 1kg of the aqueous layer after separating hyodeoxycholic acid, add 2kg of petroleum ether, adjust the pH to 9.0, stir for 30min, let it stand for 2h, remove the petroleum ether layer; add 1kg of ethyl acetate to the aqueous layer, adjust the pH to 5 .5, stir for 30min, let stand for 6h, separate the water layer, add 100g of water to the ethyl acetate layer, wash with sodium carbonate solution to pH7.2, and separate the water layer; Concentrate under pressure to 300g to stop the concentration, add 900g of water, add 10% sodium hydroxide solution to adjust the pH to 9.0, heat to 70°C, and take a sample to detect that the concentration of chenodeoxycholic acid is 23mg / mL; 3. Complexation: According to goose Calculation of the concentration of oxycholic acid The amount of magnesium carbonate added is 27.6g, add 27.6g of water, dissolve the magnesium salt to form a solution, add the magnesium salt solution while stirring, finish adding within 4h, keep warm ...

Embodiment 2

[0020] 1. Extraction: Add 1kg of hyodeoxycholic acid to the aqueous layer, add 3kg of petroleum ether, adjust the pH to 9.2, stir for 30min, let stand for 2h, remove the petroleum ether layer; add 1kg of ethyl acetate to the aqueous layer, adjust the pH to 6 .0, stirred for 30min, stood for 8h, separated to remove the water layer, added 100g of water to the ethyl acetate layer, washed with sodium bicarbonate solution to pH7.4, and separated to remove the water layer; 2. Concentration: the ethyl acetate layer, usually Stop the concentration when the pressure is concentrated to 300g, add 900g of water, add 10% sodium hydroxide solution to adjust the pH to 9.5, heat to 72°C, take a sample to detect the concentration of chenodeoxycholic acid 25.1mg / mL; 3. Complexation: According to The concentration of chenodeoxycholic acid calculates that the amount of magnesium chloride is 30.12g, add 36g of water, dissolve the magnesium salt to form a solution, add the magnesium salt solution wh...

Embodiment 3

[0022]1. Extraction: Add 1kg of the aqueous layer after separating hyodeoxycholic acid, add 4kg of petroleum ether, adjust the pH to 9.5, stir for 30min, let stand for 2h, and remove the petroleum ether layer; add 1kg of ethyl acetate to the aqueous layer to adjust pH6.5, stirred for 30min, stood still for 8h, separated to remove the water layer, added 100g water to the ethyl acetate layer, added 1% ammonia solution to wash to pH7.5, and separated to remove the water layer; 2. Concentration: the ethyl acetate layer, Concentrate at normal pressure to 300g, stop the concentration, add 900g of water, add 10% sodium hydroxide solution to adjust the pH to 10, heat to 70-75°C, take a sample to detect the concentration of chenodeoxycholic acid 22.7mg / ml; 3. Complexation: According to the concentration of chenodeoxycholic acid, the amount of magnesium sulfate required is 27.2g, add 40.8g of water, dissolve the magnesium salt to form a solution, add the magnesium salt solution while sti...

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Abstract

The invention relates to a method for preparing chenodeoxycholic acid by an extraction complexing process. The method comprises the following steps: 1, extracting; 2, concentrating; 3, complexing; 4,removing magnesium; 5, crystallizing; 6, recrystallizing for obtaining the chenodeoxycholic acid finished product. According to the method, impurities such as sterols and proteins in chenodeoxycholicacid are extracted with petroleum ether, then ethyl ester is washed with weak alkaline water to remove hyocholic acid impurities in chenodeoxycholic acid, chenodeoxycholic acid is easy to complex under high-temperature catalysis of ethyl acetate, and complete separation of chenodeoxycholic acid is achieved. The method has the beneficial effects that the yield is high and is 20-25%, the melting point is high and is 160-170 DEG C, and the content of high-purity products is 98% or above through HPLC detection. The method has the characteristics of simplicity in operation, short process flow, reduction of organic reagent consumption, cost saving, safety, environmental protection and the like.

Description

technical field [0001] The invention belongs to the technical field of separation and extraction of natural products, and in particular relates to a method for preparing chenodeoxycholic acid by extraction and complexation. Background technique [0002] Chenodeoxycholic acid (3α, 7α-dihydroxy-5β-cholanic acid) Chenodeoxycholic Acid (CDCA for short) has the effects of relieving asthma, resolving phlegm, antitussive and anti-inflammation, and its choleretic effect is particularly significant. Cholesterol absorption, synthesis, and reduction of cholesterol in the bile, thereby inhibiting the formation of cholesterol stones and promoting their dissolution, and can effectively reduce cholesterol saturation. 1. Treatment of cholesterol-type stones. CDCA can inhibit the activity of HMG-COA reductase; stimulate the activity of bile acid synthesis rate-limiting enzyme, thereby expanding the bile acid pool to facilitate the dissolution of cholesterol in micellar state. The best effe...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 赵厚发郭庆徐宾朋
Owner ANHUI KEBAO BIOLOGICAL ENG CO LTD
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