Method for separating and purifying chenodeoxycholic acid from duck gall

A technique for chenodeoxycholic acid and duck bile is applied in the field of separation and purification of chenodeoxycholic acid, which can solve the problems of inability to obtain chenodeoxycholic acid, and achieve the effect of improving extraction efficiency.

Active Publication Date: 2012-12-19
苏州天绿生物制药有限公司 +1
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chenodeoxycholic acid in chicken bile is about 80%, the content is high, and the extraction is simple. The traditional solvent extraction method can obtain chenodeoxycholic acid with a high purity (above 96%), while chenodeoxycholic acid in duck bile The content of cholic acid is about 40~50%. The traditional solvent extraction method cannot obtain chenodeoxycholic acid with higher purity. It is necessary to develop a new purification method according to its characteristics.

Method used

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  • Method for separating and purifying chenodeoxycholic acid from duck gall
  • Method for separating and purifying chenodeoxycholic acid from duck gall
  • Method for separating and purifying chenodeoxycholic acid from duck gall

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1 prepares duck gall paste crude product from duck gall

[0029] Take 50kg of fresh duck bile (volume 50L) and put it in a stainless steel reaction kettle, add sodium hydroxide according to the amount of bile 50g / L, that is, add 2.5kg sodium hydroxide, heat and boil for 24 hours for saponification, and the mass percentage is 38 % concentrated hydrochloric acid to adjust the pH to 2, crystallize to obtain about 5 kg of brown paste, dissolve the paste with 50 kg of ethanol, add 0.5 kg of activated carbon to reflux for decolorization for 2 hours, filter to remove activated carbon, evaporate and concentrate to recover ethanol, and concentrate to obtain Duck gall paste crude product 5kg.

Embodiment 2

[0030] Embodiment 2 Calcium salt method prepares chenodeoxycholic acid crude product

[0031] 100kg of fresh duck bile is placed in a stainless steel reaction kettle, and sodium hydroxide is added according to the bile amount of 50g / L, that is, 5kg of sodium hydroxide is added, heated and boiled for 24 hours for saponification, and then calcium chloride with 5% of the bile weight is added, i.e. 5kg Calcium chloride, the total cholic acid calcium salt was precipitated, and the filtrate was discarded by centrifugation to obtain the total cholic acid calcium salt. The total cholic acid calcium salt is washed with 40kg of water, the water-insoluble matter is discarded, the pH of the aqueous solution is adjusted to 2 with 17-20% hydrochloric acid, and the crude chenodeoxycholic acid is precipitated, filtered, and dried to obtain the crude chenodeoxycholic acid .

Embodiment 3

[0032] Example 3 Separation and Purification of Chenodeoxycholic Acid

[0033] 1) Dissolution and extraction: Weigh 100g of the crude product of duck gall paste obtained in Example 1, add 500g of chloroform, 500g of methanol, and 500g of water, heat and reflux for 1 hour, after it is completely dissolved, cool to 25°C, and let it stand for stratification. Obtain the chloroform phase and the methanol / water phase, evaporate and recover the methanol, adjust the pH of the remaining water phase to 2 with hydrochloric acid with a mass percentage of 17-20%, crystallize, and centrifuge to obtain chenodeoxycholic acid product A;

[0034] 2) Ethyl acetate extraction: Dissolve chenodeoxycholic acid product A in 5% sodium hydroxide solution with 5 times the mass, cool to 20°C, add ethyl acetate in an amount of chenodeoxycholic acid product A per gram Add 5ml, adjust the pH to 7.2, separate layers to obtain ethyl acetate phase, continue to add ethyl acetate to the water layer, the amount a...

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Abstract

The invention provides a method for separating and purifying chenodeoxycholic acid from duck gall, and concretely comprises to the following steps: dissolving and extracting a duck gall paste crude product, extracting ethyl acetate, and ultrafiltering and removing impurities. The method has the following advantages that 1) the raw material source of chenodeoxycholic acid can be enlarged, the method for separating and purifying chenodeoxycholic acid from the duck gall is provided; and 2) the content of chenodeoxycholic acid extracted from the duck gall by a traditional method is low with about 60%. The HPLC content of chenodeoxycholic acid obtained by using the method of the invention can reach more than 96%, and the extraction efficiency of chenodeoxycholic acid is enhanced.

Description

technical field [0001] The invention relates to biochemical separation and purification, in particular to a method for separating and purifying chenodeoxycholic acid from duck bile. Background technique [0002] Chenodeoxycholic acid (3α,7α-dihydroxy-5β-cholic acid, Chenodeoxycholic Acid, referred to as CDCA) has the effect of correcting cholesterol-saturated bile. In 1972, the treatment of dissolving cholesterol gallstones was officially developed by the United Kingdom, and chenodeoxycholic acid was used as the first drug to correct saturated bile and dissolve gallstones. It is now known that chenodeoxycholic acid is contained in the bile, liver, kidney and other tissues of many animals and humans. [0003] Chenodeoxycholic acid can also be used as an intermediate in the synthesis of ursodeoxycholic acid (3α,7β-dihydroxy-5β-cholanic acid) and other steroidal compounds. Ursodeoxycholic acid can promote the secretion of bile solid components. It is a powerful choleretic dru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 陆其华周大海
Owner 苏州天绿生物制药有限公司
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