Method for preparing cholic acid
Ethanol crystallization
Preparation of crude bovine bile acid Take bovine or sheep bile, add 100 g and L sodium hydroxide, steam for 12-18 h, and get a saponification solution. Right after cooling, acid is put into adapt pH 1, and bile acid is brought on, and bile acid is taken out, boiled, washed, dried at 75 ° C, and ground to obtain crude bovine bile acid.
Bovine, choline acid [NaOH] → [100 ° C, 12-18h] saponification solution [H2SO4] → [pH1, 75 ° C] crude cattle, choline
Preparation of meat and sheep bile acid preparation Take crude bile acid, add 0. 5-1 times of 95% ethanol, heat to reflux until the solid dissolves, and cool. The crystals were taken out and smashed, filtered, and washed with 95% ethanol until the filtrate was colorless. Add 4x of ethanol to the crystal, add 100-150g/L activated carbon, heat to reflux until the amazingly is dissolved, filter while hot, concentrate the filtrate to 1/4 of the original volume, cool, crystallize, filter, add ethanol to wash and crystallize, and dry. Beef and lamb bile acid products.
Primitive cattle, choline acid [ethanol, activated carbon] → refined liquid [90 ° C or less] → completed product of cattle and choline
Ethyl acetate splitting up
Preparation of crude pig cholic acid Take fresh pig bile, add 3-3. 5 times of overloaded lime water clear solution under stirring, continue to stir for 5-10min after heating, heat to cooking for 2min, cool, filter, filtrate and hydrochloric acid solution At pH 3. 5, the precipitate was precipitated and allowed to remain for 12 h or more to obtain primitive bile acid. Take out there, wash with water, add 1. 5 times salt hydroxide, add 9 times water, heat and steam for 12-18h, let cool, let stand overnight, get a paste. Add water, add sulfuric acid to adjust pH 1, and precipitate choline acid. Get rid of, mash, rinse to no acid and filter to obtain crude choline.
This Halloween bile [saturated lime water] → [100 ° C, ph level 11-12] alkaline filtrate [HCl] → [pH 3. 5] crude bile acidity [water, NaOH] → paste [H2SO4] → [pH1] crude pig cholic acid
Preparation of pig bile acid finished product Take crude pig bile acid, add 4x of ethyl acetate, add 150-200g/L activated carbon, heat reflux for 0. 5h, let cool, filter, filter cake plus 1. 5-2. 5 times ethyl acetate treatment 1 Once, the filtrate was combined twice. After adding 200 g/L of anhydrous sodium sulfate, it was allowed to remain overnight, concentrated to 1/3 of the original quantity, discharged, cooled, crystallized, strained, washed with ethyl acetate, and dried to obtain a finished product of porcine cholic acid.
Primitive pig cholic acid [ethyl acetate, activated carbon] → filtrate [anhydrous sodium sulfate] → filtrate [concentrated] → pig cholic acid finished product.
Pet extraction
Extracted from the bile of livestock (pig, cattle, sheep, rabbit).
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