Separation purification preparation method of chenodeoxycholic acid in pig's bile

A technology for separation and purification of chenodeoxycholic acid, applied in the field of preparation of chenodeoxycholic acid, can solve the problems of inapplicability, unsafe organic solvents, low yield, etc., achieve low cost, easy industrial production, and simple operation Effect

Inactive Publication Date: 2006-11-29
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0005] Chenodeoxycholic acid is mainly extracted from the bile of poultry or animal bile. The traditional extraction and preparation process is complicated, the yield is low, and a large amount of unsafe organic solvents are used (Pharmaceutical Industry, 1987, 18 (9), 416; Application Technology, 1998, 429-10; US patent, 4,331,607; US patent 4,163,017) cannot apply to the requirements of modern industry

Method used

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Examples

Experimental program
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Embodiment Construction

[0028] Take fresh or frozen pig bile, add lime milk (lime: water = 1: 12) or lime water (lime: water = 1: 30) to remove bilirubin, add 40% of its volume of solid hydrogen to the filtered mother liquor Sodium oxide, heating and boiling for 24 hours, after saponification, adjust the pH to 2-3 with hydrochloric acid (20%), filter and wash with water until neutral to obtain total cholic acid.

[0029] Dissolve the total bile acid in 3 times the amount of absolute ethanol, add 0.5-1% activated carbon, raise the temperature and reflux for 30 minutes, filter while it is hot, extract the filtrate with petroleum ether several times, and combine the extracts.

[0030] Add 5% NaOH-ethanol solution equal to the volume of the extract, add it into the degreased solution under stirring, heat up and reflux for 2 hours, cool down to room temperature, adjust the pH to 8-8.5 with hydrochloric acid (20%), and then add 15% etc. volume of Bacl 2 Aqueous solution, continue to reflux for 2 hours, ad...

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Abstract

A process for separating the chenodeoxycholic acid from pig's gall and purifying it includes such steps as preparing general cholic acid from the mother liquid generated by extracting the cholerythrin from pig's gall, saponifying, regulating pH value to obtain crude chenodeoxycholic acid, decoloring, defatting, preparing the deposit of barium chenodeoxycholate, reacting on potassium carbonate to remove Ba, regulating pH value, and purifying by silicon gel column.

Description

technical field [0001] The invention relates to a preparation method of chenodeoxycholic acid (3α, 7α-dihydroxy-5β-cholanic acid), and mainly relates to a method for extracting chenodeoxycholic acid from pig bile. Background technique [0002] Chenodeoxycholic acid (3α, 7α-dihydroxy-5β-cholanic acid) Chenodeoxycholic Acid (CDCA for short), first discovered in goose bile in 1824, in 1924, Wieland and Windaus in different bile (human and goose) Chenodeoxycholic acid, the most soluble bile acid, was found in chenodeoxycholic acid and was named chenodeoxycholic acid. [0003] Chenodeoxycholic acid has the effects of relieving asthma, resolving phlegm, antitussive and anti-inflammation, and its choleretic effect is particularly significant. It reduces the cholesterol in the bile by reducing the absorption and synthesis of cholesterol, thereby inhibiting the formation of cholesterol stones and promoting their dissolution. , and can effectively reduce cholesterol saturation. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00A61K35/413
Inventor 孟艳秋张力
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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