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Method for separating hyodeoxycholic acid from pig gall paste by extraction method

A technology of hyodeoxycholic acid and pig bile ointment, which is applied in the directions of steroids and organic chemistry, can solve the problems of high production cost, large amount of organic reagents, easy decomposition, etc., and achieve the effect of shortening the production cycle

Inactive Publication Date: 2020-11-20
ANHUI KEBAO BIOLOGICAL ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethyl acetate method is a traditional method with a low yield of 10%-15%, low purity (melting point 170-190°C), large amount of organic reagents, ethyl acetate is volatile and easy to decompose when heated, which affects the quality of the product during the extraction process Very large, high production cost, complex operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a laboratory test, weigh 1 kg of pig gall paste, add 8 kg of methanol, add 80 g of concentrated sulfuric acid, heat and reflux for 4 hours, add calcium bicarbonate while it is hot to neutralize to pH 7.0, filter, and collect the filtrate; heat the filtrate to 80 ℃, vacuum 0.08MPa to concentrate and recover methanol until no methanol flows out, it becomes viscous, and weighs 650g; add 1850g cyclohexane, stir for 60min, let stand for 4h, separate and remove the lower layer; add 1850g cyclohexane to the lower layer, stir 30min, let it stand for 2h, and remove the lower layer; add 1850g of cyclohexane to the lower layer again, stir for 10min, let it stand for 1h, and remove the lower layer; the combined cyclohexane layer is washed with saturated sodium bicarbonate solution to pH7.0, and left standing Separate the water layer; remove the cyclohexane layer, recover the cyclohexane to 1300g, stop concentrating, lower the temperature, cool and crystallize, and filter to obtai...

Embodiment 2

[0023] In a laboratory test, weigh 1 kg of pig gall paste, add 9 kg of methanol, add 90 g of concentrated sulfuric acid, heat to reflux for 5 hours, add calcium bicarbonate while it is hot to neutralize to pH 7.1, filter, and collect the filtrate; heat the filtrate to 60 ℃, vacuum 0.07MPa to concentrate and recover methanol until no methanol flows out, it becomes viscous, and weighs 700g; add 2100g of pentane, stir for 60min, let it stand for 4h, separate and remove the lower layer; add 2100g of pentane to the lower layer, stir for 30min, Let stand for 2h, separate to remove the lower layer; add 2100g of pentane to the lower layer again, stir for 10min, let stand for 1h, separate to remove the lower layer; combine the pentane layer and wash with saturated sodium bicarbonate solution to pH 7.0, let stand and separate to remove the water layer ; When the pentane layer is recovered to 1400g, stop concentrating, cool down, cool and crystallize, and filter to obtain 330g of methyl h...

Embodiment 3

[0025] In a laboratory test, weigh 1 kg of pig gall paste, add 10 kg of methanol, add 100 g of concentrated sulfuric acid, heat to reflux for 6 hours, add calcium bicarbonate while it is hot to neutralize to pH 7.3, filter, and collect the filtrate; heat the filtrate to 80 ℃, vacuum 0.08MPa to concentrate and recover methanol until no methanol flows out, it becomes viscous, and weighs 750g; add 2250g of petroleum ether, stir for 60min, let stand for 4h, separate and remove the lower layer; add 2250g of petroleum ether to the lower layer, and stir for 30min , stand still for 2h, and remove the lower layer; add 2250g of petroleum ether to the lower layer again, stir for 10min, let stand for 1h, and remove the lower layer; the combined petroleum ether layer is washed with saturated sodium bicarbonate solution to pH7.2, and then separated by standing water layer; the petroleum ether layer, when the petroleum ether is recovered to 1500g, stop concentrating, cool down, cool and cryst...

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PUM

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Abstract

The invention relates to a method for separating hyodeoxycholic acid from pig gall paste by an extraction method. The method comprises the following steps: 1, esterification of pig gall paste; 2, concentrating; 3, extraction; 4, concentrating and crystallizing; 5, hydrolytic acidification; 6, drying; 7, crystallizing, filtering and drying to obtain a hyodeoxycholic acid finished product. The method has the advantages that the yield is high and up to 20%-30% (the yield of a traditional method is 10%-15%); the purity is high, and the melting point is 200-204 DEG C (the melting point of the traditional method is 170-190 DEG C); the production period is shortened, and the use amount of an organic solvent is small (the use amount of the traditional method is large); and the product is white powder in appearance(faint yellow or yellow powder in the traditional method).

Description

technical field [0001] The invention relates to a method for extracting hyodeoxycholic acid in animal bile, in particular to a method for separating hyodeoxycholic acid in pig bile paste by extraction. Background technique [0002] Hyodeoxycholic acid is a cholic acid extracted from pig bile. It can be used as an anti-inflammatory drug to treat chronic bronchitis, hyperlipidemia, atherosclerosis, etc. This product can stimulate the secretion of bile and make the bile thinner without increasing the amount of solids. It is suitable for cholangitis, cholecystitis, cholelithiasis and other non-obstructive cholestasis; it can also accelerate the gallbladder contrast medium to be discharged from the liver and contribute to imaging. It can still promote the decomposition of intestinal fat and the absorption of fat-soluble vitamins, and can be used for indigestion caused by liver and gallbladder diseases. At the same time, it is also the main raw material for preparing artificial b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 郭庆徐宾朋赵露
Owner ANHUI KEBAO BIOLOGICAL ENG CO LTD
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