Method for removing hyocholic acid from chenodeoxycholic acid
A technology of chenodeoxycholic acid and hyocholic acid, applied in the field of removing hyocholic acid, can solve the problems of poor effect, high cost, low efficiency, etc., achieve good separation effect and reduce volatilization
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Embodiment 1
[0013] Take 120 kg of crude chenodeoxycholic acid extracted from pig bile (HPLC content 61.3%, see attached table 1 for specific detection indicators) that has been crudely separated and deoiled, put it into a 1000L enamel extraction kettle, add 600 kg of butyl acetate, Reflux for 1 hour after heating to boiling, add 12 kg of activated carbon, continue to stir and reflux for 1 hour, and then pass through a titanium rod filter unit for heat preservation and filtration to obtain a chenodeoxycholic acid butyl acetate solution.
[0014] Pump the chenodeoxycholic acid butyl acetate solution into a 1000L enamel precipitation kettle, cool to 40°C, add 12 kg of sec-butylamine, keep stirring for 1 hour, cool to room temperature 25°C, and crystallize for 4 hours to obtain a mixed suspension Cloudy liquid.
[0015] Put the mixed suspension into a D800 clean and sealed stainless steel centrifuge for centrifugation, and obtain chenodeoxycholic acid ammonium salt and butyl acetate mother li...
Embodiment 2
[0019] Take 110 kg of crude chenodeoxycholic acid extracted from pig bile (HPLC content 59.7%, see attached table 1 for specific detection indicators) that has been crudely separated and deoiled, and put it into a 1000L enamel extraction kettle, add 540 kg of butyl acetate, and heat Reflux for 1 hour after boiling, add 10 kg of activated carbon, continue to stir and reflux for 1 hour, and then pass through a titanium rod filter unit for heat preservation and filtration to obtain a chenodeoxycholic acid butyl acetate solution.
[0020] Pump the chenodeoxycholic acid butyl acetate solution into a 1000L enamel precipitation kettle, cool to 40°C, add 11 kg of sec-butylamine, keep stirring for 1 hour, cool to room temperature 25°C, and crystallize for 4 hours to obtain a mixed suspension Cloudy liquid.
[0021] The mixed suspension was put into a D800 clean and sealed stainless steel centrifuge, and centrifuged to obtain ammonium chenodeoxycholate and butyl acetate mother liquor, w...
Embodiment 3
[0025] Take 125 kg of crude chenodeoxycholic acid extracted from pig bile (HPLC content 63.3%, specific test indicators see attached table 1) that has been crudely separated and deoiled, and put it into a 1000L enamel extraction kettle, add 625 kg of butyl acetate, and heat Reflux for 1 hour after boiling, add 12.5 kg of activated carbon, continue to stir and reflux for 1 hour, then pass through a titanium rod filter unit for heat preservation and filtration to obtain a chenodeoxycholic acid butyl acetate solution.
[0026] Pump the chenodeoxycholic acid butyl acetate solution into a 1000L enamel precipitation kettle, cool to 40°C, add 12.5 kg of sec-butylamine, keep stirring for 1 hour, cool to room temperature 25°C, and crystallize for 4 hours to obtain a mixed suspension Cloudy liquid.
[0027] Put the mixed suspension into a D800 clean and sealed stainless steel centrifuge for centrifugation to obtain chenodeoxycholic acid ammonium salt and butyl acetate mother liquor, whe...
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