Method for extracting cholic acid of ducks and chenodeoxycholic acid (CDCA) from bile of ducks
A technique for chenodeoxycholic acid and duck cholic acid, which is applied in the field of preparation of chenodeoxycholic acid, can solve the problems of slow precipitation, complicated process and low efficiency, and achieves the effects of easy operation and simple preparation method.
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Embodiment 1
[0031] A method for extracting duck cholic acid and chenodeoxycholic acid from duck bile, comprising the following steps:
[0032] A, Extraction of Crude Bile Acids
[0033] Take 1000g of fresh duck bile and put it into the reaction kettle, add 0.35 times the amount of sodium hydroxide, continue to put in, seal and keep the pressure, heat up to 120°C, stir for 12 hours, let it stand down to room temperature, add dilute hydrochloric acid to adjust the pH value to 3 to get a black paste Material 200g. Add 3 times the amount of methanol to the black paste, heat to 50°C, stir until completely dissolved; continue to add 3 times the amount of petroleum ether and stir for 30 minutes, let it stand, siphon to remove the petroleum ether layer; continue to add 3 times the amount of petroleum ether , and repeat 2 more times; concentrate the petroleum ether layer to recover petroleum ether, and the concentrate is grease, which is discarded. The methanol layer was concentrated in vacuo be...
Embodiment 2
[0039] A method for extracting duck cholic acid and chenodeoxycholic acid from duck bile, comprising the following steps:
[0040] A, Extraction of Crude Bile Acids
[0041] Take fresh duck bile and put it into the reaction kettle, continue adding 0.3 times the amount of sodium hydroxide, seal and keep the pressure and raise the temperature to 125°C, stir and react for 12 hours, let it stand at room temperature, add dilute hydrochloric acid to adjust the pH value to 2.8 to get a black paste . Add 4 times the amount of methanol to the black paste, heat to 50°C, stir until completely dissolved; continue to add 3 times the amount of petroleum ether and stir for 30 minutes, let it stand, siphon to remove the petroleum ether layer; continue to add 3 times the amount of petroleum ether , and repeat 3 times; concentrate the petroleum ether layer to recover petroleum ether, and the concentrate is grease, which is discarded. The methanol layer was concentrated in vacuo below 70°C to ...
Embodiment 3
[0047] A method for extracting duck cholic acid and chenodeoxycholic acid from duck bile, comprising the following steps:
[0048] A, Extraction of Crude Bile Acids
[0049] Take fresh duck bile and put it into the reaction kettle, continue adding 0.4 times the amount of sodium hydroxide, seal and keep the pressure and raise the temperature to 115°C, stir and react for 13 hours, let it stand to cool down to room temperature, add dilute hydrochloric acid to adjust the pH to 2.8 to get a black paste . Add 3 times the amount of methanol to the black paste, heat to 50°C, stir until completely dissolved; continue to add 3 times the amount of petroleum ether and stir for 30 minutes, let it stand, siphon to remove the petroleum ether layer; continue to add 3 times the amount of petroleum ether , and repeat 2 more times; concentrate the petroleum ether layer to recover petroleum ether, and the concentrate is grease, which is discarded. The methanol layer was concentrated in vacuo be...
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