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Method for extracting hyodeoxycholic acid from pig bile

A technology for hyodeoxycholic acid and pig bile paste, which is applied in the directions of steroids, organic chemistry, etc., can solve the problems of great influence on the quality of hyodeoxycholic acid, complicated operation of the extraction method, influence on environmental quality, etc., and it is easy to achieve the reaction conditions. Control, small amount of solvent, the effect of avoiding contamination

Active Publication Date: 2013-04-03
SICHUAN DAXIONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional extraction method of hyodeoxycholic acid, a large amount of organic solvent ethyl acetate is used for extraction and then decolorized with activated carbon. However, due to the volatility of the organic solvent ethyl acetate, it is easy to decompose when heated. The quality of the acid has a great influence; and the traditional extraction method is complicated to operate and the production cost is high; at the same time, the volatilization of ethyl acetate will affect the environmental quality

Method used

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Embodiment 1

[0019] Step 1: Take 200g of pig gallbladder paste, add 1600mL of water, 200g of sodium hydroxide, stir to dissolve, heat to boiling, keep stirring for 10h, let stand to cool to room temperature, remove the upper layer of yellow-brown clear night, and the lower layer is black viscous material . Sodium hydroxide is added for saponification reaction, and the bile acid in the bound form in the pig bile ointment is changed into the sodium salt of bile in the free form.

[0020] Step 2: Add 20 mL of hydrogen peroxide to the black viscous material, stir and decolorize for 5 hours, to ensure that the hydrogen peroxide oxidizes the pigment and removes the pigment. Decolorization with hydrogen peroxide under alkaline conditions after saponification not only achieves convenient process operation but also saves time.

[0021] Step 3: Add 1600 mL of water to the previous step and stir to dissolve, adjust the pH to 6.5 with dilute sulfuric acid, and then adjust the pH to 8.5 with ammonia w...

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Abstract

The invention discloses a method for extracting hyodeoxycholic acid from pig bile, which comprises the following steps: diluting the pig bile, adding sodium hydroxide to perform the saponification reaction and removing yellowish-brown supernatant; adding hydrogen peroxide to carry out decoloring; regulating pH, heating to the temperature of 50 DEG C, adding magnesium salt solution, stirring, crystallizing, filtering and collecting solid; adding sodium carbonate into the solid, stirring to enable the solid to be dissolved, filtering and collecting filtrate; and adding dilute sulphuric acid into the filtrate to regulate pH to 3, carrying out filter pressing, washing a filter cake to pH of 6 to 7, drying and grinding to obtain a hyodeoxycholic acid pure product. According to the invention, the method adopts inorganic salt and magnesium salt to crystallize and separate the hyodeoxycholic acid without adopting an organic solvent to carry out extraction; the use quantity of the magnesium salt is 0.15 time of mass of the pig bile; the use quantity of the solvent is small; cost is low; quality of the hyodeoxycholic acid is prevented from being influenced due to volatilization of the organic solvent; pollution to the environment, which is caused by the organic solvent, is avoided; the method has a simple process and few operating steps and the reaction conditions of each step is easy to control; and the purity of the hyodeoxycholic acid can reach over 99 percent.

Description

technical field [0001] The invention relates to a method for extracting hyodeoxycholic acid, in particular to a method for extracting hyodeoxycholic acid from pig bile ointment. Background technique [0002] Hyodeoxycholic acid (HDCA) is a hypolipidemic drug, which can inhibit the formation of cholic acid and dissolve fat, reduce blood cholesterol and triglycerides, and is suitable for type I a or I b hyperlipidemia and atherosclerosis. Hyodeoxycholic acid is an important raw material for artificial bezoar formula. In actual production, hyodeoxycholic acid with a purity of ≥99.0% is required. In the traditional extraction method of hyodeoxycholic acid, a large amount of organic solvent ethyl acetate is used for extraction and then decolorized with activated carbon. However, due to the volatility of the organic solvent ethyl acetate, it is easily decomposed by heat. The quality of the acid has a great influence; and the traditional extraction method is complicated to operate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 梁万超吴眉平刘建英
Owner SICHUAN DAXIONG BIOTECH
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