Non-organic solvent extraction method for chenodeoxycholic acid in bird gall
A chenodeoxycholic acid, non-organic technology, applied in the field of extraction of chenodeoxycholic acid, can solve the problems of complex extraction process, environmental pollution and high production cost
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Embodiment 1
[0007] Embodiment 1: take poultry gall, chop, filter, add 5% sodium hydroxide of bile mass, stir and dissolve, heat and boil to carry out saponification reaction, time 20 hours; Saponification solution adds 10% hydrochloric acid solution to neutralize and adjust pH to 2 , stir, stand still, filter, and collect the precipitated total bile acids; add 5% sodium hydroxide solution to dissolve the total bile acids, add 10% of its mass of activated carbon, heat and reflux for 1 hour for decolorization, and add 10% of mass of chlorinated bile acids to the filtrate Calcium, keep stirring, stand still, collect the precipitate; add 10% sodium carbonate to the calcium salt precipitate, heat and reflux for 1 hour to decalcify; filter, adjust the pH2 of the filtrate with 5% hydrochloric acid solution, stand still, filter, collect the precipitate, and vacuum dry , the crude product of chenodeoxycholic acid was obtained with a purity of 52% (HPLC).
Embodiment 2
[0008] Example 2: Take poultry bile, add 5% of its mass of sodium hydroxide, stir to dissolve, heat and boil for saponification reaction for 22 hours; add 10% hydrochloric acid to the saponification solution to neutralize and adjust pH to 3, stir, and let stand , filtered, and the precipitate was collected to obtain the total bile acid; the total bile acid was dissolved in 5% sodium hydroxide solution, and then 10% of its mass of activated carbon was added, heated to reflux for decolorization for 1 hour, and the filtrate was added with 12% of its mass of calcium chloride, continuously Stir, stand still, and collect the precipitate; add 10% sodium carbonate to the calcium salt precipitate, heat and reflux for 2 hours, decalcify, filter, adjust the pH3 of the filtrate with 7% hydrochloric acid solution, let stand, filter, collect the precipitate, and vacuum dry to obtain Chenodeoxycholic acid crude product, purity 52.8% (HPLC).
Embodiment 3
[0009] Embodiment 3: Take poultry bile, add its mass 5% sodium hydroxide, stir to dissolve, heat and boil for saponification reaction, time is 24 hours; saponification solution is added with 10% hydrochloric acid solution to neutralize and adjust Ph4, stir, stand still, filter , collect the precipitate to get the total bile acid; add 5% sodium hydroxide solution to dissolve the total bile acid, then add 10% of its mass of activated carbon, heat and reflux for decolorization for 1 hour, add 14% of its mass of calcium chloride to the filtrate, and keep stirring. Stand still and collect the precipitate; add 15% sodium carbonate to the calcium salt precipitate, heat and reflux for 3 hours, and decalcify; filter, and adjust the pH of the filtrate to 3.5 with 10% hydrochloric acid solution, let stand, filter, collect the precipitate, and dry in vacuum to obtain goose Deoxycholic acid crude product, purity 56.89% (HPLC).
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