Method for extracting bile acid from bilirubin leftovers

A technology for leftovers and bile acids, applied in the direction of steroids, organic chemistry, etc., can solve the problems of low product purity, complicated operation, inconspicuous stratification, etc., and achieve the effect of high product purity and simple operation.

Inactive Publication Date: 2012-05-09
娄倩倩 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The disadvantages of the above two methods are: although all the proteins in the bile can be removed, cholesterol and neutral fat are still retained in the bile acid, so the product has a low purity
The disadvantages of this method are: complex operation, large amount of methanol, no obvious stratification when extracting cholesterol with chloroform and methanol, difficult to master, prone to errors, difficu...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 500 kg of leftover bile paste for extracting bilirubin was pulverized and added to a reaction tank. Then add 10% sodium hydroxide solution of 10 times the volume of gall paste, and heat to 100°C. Start timing after the gallbladder dissolves, heat, reflux, and react for 12 hours. Then, after the liquid is cooled to 80°C and the reaction liquid is separated, siphon out the upper liquid, add 10 times the volume of the liquid in water to dissolve it, and after it is completely dissolved, add hydrogen peroxide that is 2 times the volume of the upper liquid to oxidize, and let it stand for 12 hours . After the oxidation is completed, filter the clear liquid, adjust its pH value with 30% hydrochloric acid solution, and add hydrochloric acid under constant stirring to precipitate bile acid crystals. When the pH reaches 2-3, bile acids are basically all precipitated. Then filter and wash the bile acid solids to neutrality. Removes water soluble impurities. The resulting sol...

Embodiment 2

[0027] 500 kg of leftover bile paste for extracting bilirubin was pulverized and added to a reaction tank. Then add 10% sodium hydroxide solution of 10 times the volume of gall paste, and heat to 100°C. Start timing after the gallbladder dissolves, heat, reflux, and react for 10 hours. Then, after the liquid is cooled to 60°C and the reaction liquid is separated, siphon out the upper layer liquid, add 10 times the volume of the layer liquid in water to dissolve it, and after it is completely dissolved, add 3 times the volume of the upper layer liquid in hydrogen peroxide for oxidation, and let it stand for 10 hours . After the oxidation is completed, filter the clear liquid, adjust its pH value with 30% hydrochloric acid solution, and add hydrochloric acid under constant stirring to precipitate bile acid crystals. When the pH reaches 2-3, bile acids are basically all precipitated. Then filter and wash the bile acid solids to neutrality. Removes water soluble impurities. T...

Embodiment 3

[0029] 500 kg of leftover bile paste for extracting bilirubin was pulverized and added to a reaction tank. Then add 10% sodium hydroxide solution of 10 times the volume of gall paste, and heat to 100°C. Start timing after the gallbladder dissolves, heat, reflux, and react for 14 hours. Then, after the liquid is cooled to 80°C and the reaction liquid is separated, siphon out the upper layer liquid, add 10 times the volume of the layer liquid in water to dissolve, and after it is completely dissolved, add 2 times the volume of the upper layer liquid in hydrogen peroxide for oxidation, and let it stand for 16 hours . After the oxidation is completed, filter the clear liquid, adjust its pH value with 30% hydrochloric acid solution, and add hydrochloric acid under constant stirring to precipitate bile acid crystals. When the pH reaches 2-3, bile acids are basically all precipitated. Then filter and wash the bile acid solids to neutrality. Removes water soluble impurities. The ...

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Abstract

The invention relates to a method for extracting bile acid from bilirubin leftovers. The method comprises the following steps of: adding alkali into leftovers of bile from which bilirubin is completely extracted serving as a raw material for saponifying; adding hydrogen peroxide for decolorizing; and adding an acid for separating and washing. In the invention, the aim of purifying is fulfilled by dissolving impurities such as proteins and fats in bile cream into an alkaline liquor in a high-temperature saponifying way, further removing impurities in a chemical decolorizing way and dissolving and washing out water-soluble impurities in a pH value adjusting way. The method for producing bile acid disclosed by the invention has the advantages of easiness for operating, freeness from toxic and harmful organic solvent, realization of large-scale industrial production, high product purity (bile acid is more than 98 percent), and total yield of over 40 percent.

Description

technical field [0001] The invention relates to a method for extracting bile acid. Background technique [0002] With the advancement of science and technology and the increasingly fierce competition and challenges in the research and development of new drugs at home and abroad, the focus of new drug research is increasingly shifting to the development and utilization of active ingredients in traditional Chinese medicine and natural medicines. The active ingredient of traditional Chinese medicine is the material basis for its medicinal effect, and its in-depth study is the key to the modernization of traditional Chinese medicine. [0003] Since the last century, the research on bile and bile acids has been a hot spot in the field of chemistry and medical science. The research focus has shifted from the initial separation and structure identification to the exploration of pharmacological effects, but the main object of research is free bile acids. With the development of med...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 娄倩倩籍立民
Owner 娄倩倩
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