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Method for producing high-purity chenodeoxy cholic acid from poultry and livestock bile

A chenodeoxycholic acid, high-purity technology, applied in chemical instruments and methods, steroid preparation, steroids and other directions, can solve the problems of complex process, low yield, etc., achieve simple production process, high product purity, The effect of increasing productivity

Inactive Publication Date: 2006-05-24
SHANDONG BOERDE BIOLOGICAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The whole process is relatively complicated, and steps such as calcium chloride salt formation, decalcification, and decolorization are required. The yield in industrial production is low, and the purity is 95%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take chicken bile, pulverize, filter, add equal weight of 1M sodium hydroxide solution, and carry out saponification reaction at 80°C for 30 hours; add 0.5M hydrochloric acid to adjust to PH = 3, stir for 2 hours, let stand, Centrifuge to collect the filter cake to obtain crude cholic acid. The crude cholic acid was adjusted to PH=10 with dilute 5M sodium hydroxide solution, injected into a strong basic anion exchange resin chromatography column, eluted with 5% sodium hydroxide solution, and combined by thin layer chromatography (TLC) Eluates detected as pure chenodeoxycholic acid spots. Then use an ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 3K, adjust the ultrafiltrate to PH=2 with 0.5M dilute acid, let it stand, centrifugal filter, and dry to obtain chenodeoxychol with a purity of 99.5% (as determined by HPLC). acid.

Embodiment 2

[0033] Take pig bile, pulverize, filter, add equal weight of 5M sodium hydroxide solution, and carry out saponification reaction at 110°C, the reaction time is 20 hours; add 2M hydrochloric acid to adjust to PH=2, stir for 5 hours, stand still, and centrifuge , Collect the filter cake to obtain crude cholic acid. Adjust the crude cholic acid to PH = 11 with dilute 1M sodium hydroxide solution, pour it into a weakly basic anion exchange resin chromatography column, elute with a mixed solution of 10% sodium acetate and 5% ethanol, and combine the Chromatography (TLC) detected the eluate as a pure chenodeoxycholic acid spot. Then use an ultrafiltration membrane with a molecular weight cut-off of 100K for ultrafiltration, adjust the ultrafiltrate to PH=3 with 2M dilute acid, let it stand, centrifugal filter, and dry to obtain chenodeoxycholic acid with a purity of 98% (as determined by HPLC). .

Embodiment 3

[0035] Take chicken bile, pulverize, filter, add an equal weight of 2M sodium hydroxide solution, and carry out saponification reaction at 90°C for 30 hours; add 1M hydrochloric acid to adjust the pH to 2.5, stir for 1 hour, stand still, and centrifuge , Collect the filter cake to obtain crude cholic acid. The crude cholic acid was adjusted to PH=11 with dilute 4M sodium hydroxide solution, injected into a weakly basic anion exchange resin chromatography column, eluted with a 12% ammonia solution, and combined and detected by thin layer chromatography (TLC) as Eluate of pure chenodeoxycholic acid spots. Then use an ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 10K, adjust the ultrafiltrate to PH=3 with 0.5M dilute acid, let it stand, centrifugal filter, and dry to obtain chenodeoxychol with a purity of 99% (as determined by HPLC) acid.

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Abstract

The invention discloses a method to manufacturing high purity chemocholic acid from fowl bile that belongs to refinement chemical and medicine field. It includes the following steps: a. saponification reaction: mixing the fowl bile and sodium hydroxide and reacting for 20-30 hours under the certain temperature; b. neutral reaction: adding dilute hydrochloric acid after saponification reaction and gaining raw cholic acid after filtering; c. column chromatography: adding dilute sodium hydroxide into raw cholic acid and injecting into chromatography column, uniting the eluent; super filtering: taking super filtering by super filtering film; e. gaining chemocholic acid that the purity is over 96% after adding dilute acid, filtering and drying. The invention has simple technology, high purity, low cost and environment protection.

Description

(1) Technical field [0001] The invention relates to a method for extracting chenodeoxycholic acid, in particular to a method for producing high-purity chenodeoxycholic acid from poultry bile, and belongs to the fields of fine chemical industry and medicine. (2) Background technology [0002] Chenodeoxycholic acid (CDCA for short) is one of the main active components of animal bile and is widely used in the pharmaceutical industry. The clinical pharmacological effects of chenodeoxycholic acid have the following aspects: [0003] 1. Treatment of cholesterol gallstones. CDCA can inhibit the activity of HMG-COA reductase; stimulate the activity of bile acid synthesis rate-limiting enzyme, thereby expanding the bile acid pool to facilitate the dissolution of cholesterol in micellar state. The best effect of CDCA was seen at 2 years after treatment, when 40% of the stones were soluble. [0004] 2. Antibacterial effect. The in vitro antibacterial test results of CDCA showed tha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00A61P31/00C07J75/00
Inventor 王洪钟田林焕王洪果丁建平崔世军
Owner SHANDONG BOERDE BIOLOGICAL SCI & TECH
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