Preparation method and application of seal cholic acid

A technology of seal and cholic acid, applied in the directions of steroids, organic chemistry, etc., can solve the problem of not separating and utilizing the cholic acid of seal, achieve good economic value and application prospect, alleviate the problem of insufficient supply, and be easy to industrialize production. Effect

Pending Publication Date: 2021-02-02
苏州恩泰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Liu Yanhong and others use precipitation and extraction to extract CDCA from duck gall (Liu Yanhong, Hu Xiangzheng, Extraction technology of chenodeoxycholic acid in duck gall paste [J], Journal of Tianjin University of Science and Technology, 2009, 24 (3): 43- 45), but the seal cholic acid in it has not been separated and utilized

Method used

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  • Preparation method and application of seal cholic acid
  • Preparation method and application of seal cholic acid
  • Preparation method and application of seal cholic acid

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0022] Grease removal: put 54.8kg of powdered duck gall paste into the reaction kettle, then add 160kg of n-heptane, reflux and stir for 2 hours, then reduce the temperature and suction filter and dry to obtain 45.75kg of solid.

[0023] Alkali-soluble decolorization and acidification: 6kg of sodium hydroxide is dissolved in 100kg of water, add 45.75kg of duck gall paste obtained in the previous step, stir to dissolve, then add 3kg of hydrogen peroxide, reflux and stir for 1 hour, then drop to room temperature, add 300kg ethyl acetate, adjusted to pH=2 with concentrated hydrochloric acid, and separated to obtain an ethyl acetate layer for later use.

Embodiment 1

[0025] PCA magnesium salt preparation: add 5% magnesium acetate solution 250kg to the standby ethyl acetate layer that obtains by preparation example 1 method (55kg powdery duck gall paste, PCA content 32.4%), stir 20min, then centrifuge rapidly, obtain 40kg PCA magnesium salt, content 81.2%.

[0026] PCA preparation: Add 40kg of the PCA magnesium salt obtained in the previous step into 200L water, add hydrochloric acid to dissolve and adjust the pH to 2, then add 100kg of ethyl acetate for extraction, separate the liquid, and evaporate the ethyl acetate phase to dryness; then add 50kg of acetic acid Ethyl ester and 50kg of dichloromethane were heated and dissolved, and then slowly dropped to 10°C for crystallization to obtain 11.2kg of PCA finished product with a purity of 97.4%. The nuclear magnetic resonance spectrum is as attached figure 1 .

Embodiment 2

[0028] PCA magnesium salt preparation: add 5% magnesium acetate solution 200kg to the standby ethyl acetate layer that obtains by preparation example 1 method (55kg powdery duck gall paste, PCA content 34.3%), stir 20min, then centrifuge rapidly, obtain 36kg PCA magnesium salt, content 77.1%.

[0029] PCA preparation: Add 36kg of the PCA magnesium salt obtained in the previous step into 180L water, add sulfuric acid to stir and dissolve, and adjust the pH to 1.5, then extract with 90kg of ethyl acetate, separate the liquid, and evaporate the ethyl acetate phase to dryness; then add 45kg of ethyl acetate and 45kg of dichloromethane were heated to dissolve, and then slowly lowered to room temperature at 25°C for crystallization to obtain 7.6kg of finished PCA with a purity of 94.6%.

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Abstract

The invention provides a method for selectively separating seal cholic acid from a duck bile extract, which facilitates the utilization of the seal cholic acid which is an important biological resource in the duck bile. The invention also provides a method for preparing chenodeoxycholic acid from the seal cholic acid. Therefore, the problem of insufficient supply of chenodeoxycholic acid raw materials can be alleviated, improved. and meanwhile, corresponding biological waste pollution is also avoided. The method is easy for industrial production and has very good economic value and applicationprospect.

Description

technical field [0001] The invention relates to a new method for preparing high-purity seal cholic acid from duck gall extract and the application of using seal cholic acid to prepare chenodeoxycholic acid. Background technique [0002] Cholesteric acid is a polyhydroxy steroidal carboxylic acid compound extracted from biological bile cream, among which ursodeoxycholic acid (UDCA) and chenodeoxycholic acid (CDCA) are more important. This type of compound has strong pharmacological properties and has a good curative effect on gallstones and other hepatobiliary diseases, and is one of the most widely used drugs for treating gallstones in the world. At present, CDCA is an important raw material for the artificial preparation of UDCA and other steroid drugs. The demand is far greater than the current supply. It is urgent to solve the problem of the source of product supply. [0003] Duck bile is one of the most important sources of CDCA in China. Long Kanghou and others studie...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 王飞沈东林
Owner 苏州恩泰新材料科技有限公司
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