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Method for extracting ursodesoxycholic acid

A technology of ursodeoxycholic acid and an extraction method, which is applied in the field of extraction of ursodeoxycholic acid, can solve the problems of many reaction steps, complicated processes, difficulty in large-scale production and the like, and achieves the effect of reducing the preparation cost

Inactive Publication Date: 2014-01-29
ANHUI PRINTING MECHANICAL & ELECTRICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Initially, people successfully synthesized ursodeoxycholic acid using cholic acid, deoxycholic acid, etc. as raw materials, but this method has many reaction steps, complicated process, low yield, and it is difficult to carry out large-scale industrial production

Method used

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  • Method for extracting ursodesoxycholic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Take a 250ml round bottom flask, add 10g of crude porcine total bile acid, 50ml of anhydrous methanol, 0.7ml of 98% concentrated sulfuric acid, stir and react at room temperature for 24h, the reaction is completed after TLC detection, and stop the reaction after no raw materials remain. Add anhydrous NaHCO to the system 3 Adjust the pH of the solid to neutral, filter off the inorganic salts, wash the filter cake with methanol, combine the filtrate and lotion, and recover the methanol under reduced pressure to obtain a tan viscous substance, add 50ml of water to dissolve the remaining inorganic salts, and then divide it with ether. Extract the organic matter (50ml, 30ml, 20ml) for the second time, combine the organic phases, and wash with saturated NaHCO 3 solution and saturated brine for 1 wash, anhydrous Na 2 SO 4 Dry for 2 hours, filter, distill off ether under reduced pressure to obtain 11.4 g of brown viscous substance, add 30 ml of benzene into the flask, dis...

Embodiment 2

[0038] Compared with Example 1, the steps (1), (2), (3) and (4) are the same, and the steps (5) and (6) are as follows:

[0039] (5) Combine the mother liquor obtained from the extraction of methyl hyocholic acid triacetate and the recrystallized mother liquor, and remove the solvent under reduced pressure to obtain 6.3 g of a tan viscous substance, at this time, the main component of which is methyl chenodeoxycholic acid For diacetate, add 50ml of methanol into the flask, raise the temperature to 65°C and stop heating after the viscous matter is completely dissolved. After the system naturally cools down to room temperature, let it stand in the refrigerator for 96h, and a pale yellow solid precipitates. Filter and filter the cake with ice-cold methanol After washing and drying, 2.4 g of a light yellow powder was obtained, which was recrystallized from methanol, and the solid was dried under an infrared lamp to constant weight to obtain 2.1 g of a white powder, mp 111-113°C, wh...

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Abstract

The invention discloses a method for extracting ursodesoxycholic acid. The method for extracting ursodesoxycholic acid comprises the steps of esterification, extraction, recrystallization, hydrolysis, secondary recrystallization and the like. According to the method for extracting ursodesoxycholic acid, porcine bile is taken as an extraction raw material, after bilirubin is extracted from the porcine bile, filtrate after hyodeoxycholic acid and hyocholicacid are extracted is collected, and separation is carried out to obtain the ursodesoxycholic acid; porcine bile raw material is available, so that preparation cost of the ursodesoxycholic acid is reduced; acetic anhydride is selected as an esterifying reagent in an extraction process, ursodesoxycholic acid and recrystallization refining conditions are determined, sodium hydroxide is adopted as an alkali catalyst, and total yield of the ursodesoxycholic acid is more than 15% by adopting the technologic process.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, and in particular relates to a method for extracting ursodeoxycholic acid. Background technique [0002] Bile is a product continuously secreted by human or vertebrate liver cells. It is a viscous, colored alkaline liquid with a bitter taste. Its components include bile acid, bile salt and bile pigment in addition to water, and a small amount of cholesterol. , fatty acids, lecithin, electrolytes and proteins. The more common animal bile today is generally poultry bile, pig bile, ox bile, bear bile, snake bile and so on. Bile acid is the main component of bile, accounting for about 50% to 70% of the total amount of bile. The physiological function of bile is mainly played by bile acid. When used as a drug, bile acid can be used to relieve fever, relieve spasm and cough, It can regulate blood pressure, strengthen the heart and gallbladder, inhibit bacteria and anti-inflammation, and regulate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 黄长乐
Owner ANHUI PRINTING MECHANICAL & ELECTRICAL
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