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Hyodeoxycholic acid refining method

A technology of hyodeoxycholic acid and a refining method, which is applied in the field of biochemical industry, can solve the problems of low purity of hyodeoxycholic acid, unfavorable large-scale production, unfriendly environment, etc., and achieves easy large-scale production, short cycle and broad market. Foreground effect

Active Publication Date: 2013-01-09
苏州天绿生物制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing methods for producing hyodeoxycholic acid mainly include two types, one is to crystallize the crude product after saponification, decolorization and degreasing with ethyl acetate, and this process uses a large amount of ethyl acetate, so the purity of hyodeoxycholic acid obtained is not high. High, yield is low; Another kind is the methyl esterification method, discloses a kind of method preparing high-purity hyodeoxycholic acid from pig bile in CN101037463A, and this method utilizes different bile acid methyl esters and benzene adducts in benzene Hyodeoxycholic acid is obtained by separating hyodeoxycholic acid with different solubility. The process is complex. In order to obtain high-purity products, harmful chemicals such as benzene, ether, and sulfuric acid are used, which is not friendly to the environment and is not conducive to large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of the leftovers after embodiment 1 pig bile extracts bilirubin

[0023] Take 1000mL of fresh pig bile, adjust the pH value to 12 with 5% sodium hydroxide solution, heat to boiling and keep warm for 2 hours, add 100mL of 10% calcium chloride solution under stirring, heat to boiling, pour off the supernatant after cooling, Filter to collect bilirubin calcium salt. After adding 5 times the weight of bilirubin calcium salt into water to dissolve, adding an appropriate amount of sodium metabisulfite for anti-oxidation, acidifying with dilute hydrochloric acid to a pH value of 1.5, adding chloroform to extract to obtain bilirubin crystals. In the supernatant obtained after filtering bilirubin calcium salt, add solid sodium hydroxide at 100g / L, heat and boil for 24 hours to saponify, cool and stand for stratification, siphon to remove the upper layer of light yellow liquid, and add appropriate amount of water to the precipitate Make it dissolve, acidify with dilu...

Embodiment 2

[0024] Example 2 Using the leftovers after extracting bilirubin from pig bile as raw material to refine hyodeoxycholic acid

[0025] Weigh a certain amount of leftovers prepared in Example 1, reflux with 5 times the weight of isopropanol for 2 hours, add activated carbon with 5% weight of leftovers and continue to reflux for 30 minutes, filter and drop to 50 ° C, add 15% dihydrate Calcium chloride solution is salted, lowered to 15°C, kept warm for 2 hours, and filtered to obtain white hyodeoxycholate precipitate. Heat 10 times the weight of hyodeoxycholic acid in drinking water to dissolve it at 50°C, slowly adjust the pH value to 3 with dilute hydrochloric acid, precipitate white crude hyodeoxycholic acid I, filter and dry (the drying temperature is 75°C). Weigh a certain amount of crude hyodeoxycholic acid I, add 5 times the weight of ethylene glycol, heat and reflux for 2 hours, wait for it to completely dissolve and lower it to 25°C, slowly add purified water dropwise ther...

Embodiment 3

[0026] Example 3 Using the leftovers after extracting bilirubin from pig bile as raw material to refine hyodeoxycholic acid

[0027] Take by weighing a certain amount of leftovers prepared in Example 1, reflux with 5 times the weight of ethyl acetate for 2 hours to dissolve the leftovers, add activated carbon with 5% weight of the leftovers and continue to reflux for 30 minutes, filter and drop to 50 ° C, add 20 % calcium chloride dihydrate solution to form a salt, lowered to 15°C, kept warm for 2 hours, and filtered to obtain white hyodeoxycholate precipitate. Heat 10 times the weight of hyodeoxycholic acid in drinking water to dissolve it at 50°C, slowly adjust the pH value to 3.5 with dilute hydrochloric acid, precipitate white crude hyodeoxycholic acid I, filter and dry (the drying temperature is 75°C). Weigh a certain amount of crude hyodeoxycholic acid I, add 5 weights of glacial acetic acid, heat and reflux for 2 hours, wait for it to completely dissolve and lower it to...

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PUM

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Abstract

The invention provides a hyodeoxycholic acid refining method. The method includes: dissolving leftovers of pig's bile after bilirubin is extracted, decoloring, filtering, saponifying, salifying, adjusting pH to range from 3-4, crystallizing to obtain a crude product of hyodeoxycholic acid, and purifying the crude product to obtain a pure product of hyodeoxycholic acid. The hyodeoxycholic acid refining method has the advantages of safety, non-toxicity, simplicity and convenience in operation, low cost, short period, high product purity, easiness in massive production and the like and has wide market prospect.

Description

technical field [0001] The invention belongs to the field of biochemical industry, in particular to a method for refining hyodeoxycholic acid. Background technique [0002] Hyodeoxycholic acid, also known as isodeoxycholic acid, α-hyodeoxycholic acid, has a molecular weight of 392.58 and can be extracted from pig bile. Hyodeoxycholic acid is a blood lipid-lowering drug, which can inhibit the formation of cholic acid and dissolve fat, reduce blood cholesterol and triglyceride, and is suitable for type Ia or Ib hyperlipidemia and atherosclerosis. It has a certain antibacterial effect on pertussis bacillus, diphtheria bacillus, and staphylococcus aureus. It can stimulate the secretion of bile and dilute the bile without increasing the solid content. It is suitable for cholangitis, cholecystitis, cholelithiasis and other non-obstructive cholestasis. It can also promote the decomposition of intestinal fat and the absorption of fat-soluble vitamins. It can be used for liver and g...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 陆其华周大海
Owner 苏州天绿生物制药有限公司