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Process for preparing hyodeoxy cholic acid from pig bile paste by calcium salt method

A technology of hyodeoxycholic acid and pig gall paste, which is applied in the direction of steroids and organic chemistry, and can solve the problems of complex operation, volatile ethyl acetate, and low yield

Inactive Publication Date: 2015-02-25
ANHUI KEBAO BIOLOGICAL ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethyl acetate method is a traditional method with a low yield of 10%-15%, low purity (melting point 170-190°C), large amount of organic reagents, ethyl acetate is volatile and easy to decompose when heated, which affects product quality during the extraction process Very large, high production cost, complex operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a laboratory test, weigh 1 kg of pig gall paste, add 10 kg of water, add 1.5 kg of sodium hydroxide, heat and saponify for 20 hours, let it stand for cooling, and lower it to normal temperature; Add 0.2kg of 30% hydrogen peroxide, the oxidation time is 10h; use 10% hydrochloric acid to adjust the above oxidation solution to pH 7, add 0.2kg of calcium chloride, heat up to 90°C, stir for 2h, let stand to cool down, and centrifuge to obtain calcium salt 0.8kg; add 12kg of cyclohexane, heat and reflux for extraction for 2 hours, let stand and cool and filter, reflux and extract for 3 times, combine the filtrates, concentrate to dryness and weigh to obtain 0.3kg of dry matter; add 4.5kg of purified water to the above dry matter Decalcify with 0.09kg of sodium carbonate, raise the temperature to 85°C, react for 3 hours, let stand to cool down and filter, add concentrated sulfuric acid to the filtrate to acidify the liquid to pH 5, and filter to obtain a crude product of 0.2...

Embodiment 2

[0021] In the pilot test in the workshop, weigh 100kg of pig gall paste, add 1500kg of water, add 225kg of sodium hydroxide, heat and saponify for 22 hours, let it stand for cooling, and lower it to room temperature; take the lower layer of sediment and add water to the original volume, and add 30kg in small amounts and multiple times 30% hydrogen peroxide, the oxidation time is 12h; use 10% hydrochloric acid to adjust the above oxidation solution to pH9, add 30kg of calcium chloride, heat up to 95°C, stir for 2h, let stand to cool down, and centrifuge to obtain 85kg of calcium salt; add 1275kg The mixture of cyclohexane and pentane was heated and refluxed for 3 hours, then cooled and filtered, refluxed and extracted 3 times in total, the filtrate was combined, concentrated to dryness and weighed to obtain 40kg of dry matter; add 680kg of purified water and 20kg of dry matter to the above dry matter Sodium carbonate was used for decalcification, the temperature was raised to 95...

Embodiment 3

[0023] In large-scale production in the workshop, weigh 500kg of pig gall paste, add 7500kg of water, add 1500kg of sodium hydroxide, heat and saponify for 24 hours, let it stand for cooling, and lower it to room temperature; remove the lower layer of sediment and add water to the original volume, and add a small amount of pig The 30% hydrogen peroxide of 200kg of gallbladder weight, oxidation time is 12h; Use 15% hydrochloric acid to adjust above-mentioned oxidation solution to pH 10, add the calcium chloride of 200kg, heat up to 95 ℃, stir reaction 4h, let stand to cool down, centrifuge to obtain Calcium salt 425kg; add 8500kg of petroleum ether, heat and reflux for extraction for 4 hours, let stand and cool and filter, reflux and extract 3 times in total, combine the filtrates, concentrate to a dry weight of 228kg; add 4600kg of purified water and 136.8kg of sodium carbonate to the above dry matter Decalcify, heat up to 5°C, react for 3 hours, let stand to cool and filter wi...

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Abstract

A process for preparing hyodeoxy cholic acid from pig gall paste by calcium salt method comprises the following steps: 1, pig bile paste saponification; 2, oxidation; 3, calcium salt formation, 4, extraction, 5, decalcification, 6, crystallization, and 7, drying for preparation of the hyodeoxycholic acid. The process has the advantages that: 1, high yield of 20% to 30% (the traditional method yield is 10% to 15%), 2, high purity and melting point of 190-200 DEG C (melting point of the traditional method is 170-190 DEG C), 3, less dosage of organic solvent ethyl acetate (the dosage of organic solvent ethyl acetate of the traditional method is large), 4, white or off-white powder appearance of the product (appearance of the product of the traditional method is light yellow or yellow powder). The process has the advantages of simple operation, short process flow, reduction of the use amount of organic reagents, saving cost, safety, environmental protection and the like.

Description

technical field [0001] The invention relates to a method for extracting hyodeoxycholic acid in animal bile, in particular to a method for extracting hyodeoxycholic acid in pig bile paste by using a calcium salt method. Background technique [0002] Hyodeoxycholic acid is a cholic acid extracted from pig bile. It can be used as an anti-inflammatory drug to treat chronic bronchitis, hyperlipidemia, atherosclerosis, etc. This product can stimulate the secretion of bile and make the bile thinner without increasing the amount of solids. It is suitable for cholangitis, cholecystitis, cholelithiasis and other non-obstructive cholestasis; it can also accelerate the gallbladder contrast medium to be discharged from the liver and contribute to imaging. It can still promote the decomposition of intestinal fat and the absorption of fat-soluble vitamins, and can be used for indigestion caused by liver and gallbladder diseases. At the same time, it is also the main raw material for prepa...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 徐宾朋郭庆赵厚发
Owner ANHUI KEBAO BIOLOGICAL ENG CO LTD
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