Method for purifying chenodeoxycholic acid
A technology of chenodeoxycholic acid and a purification method, which is applied in the field of purifying chenodeoxycholic acid to achieve the effects of low organic residue, easy standardization, and large-scale industrial production
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Embodiment 1
[0033] Quantitatively weigh 1 kg of commercially available pig gall paste, put it in a 10-liter extraction tank, add 5 liters of petroleum ether, heat to 60 ° C and reflux for 3 hours, remove the petroleum ether, and repeat this operation once more to obtain crude oil that has been degreased. Gallbladder paste 850g, the 850g crude gallbladder paste was added to 5L ethyl acetate to reflux to dissolve, then add 85g activated carbon to decolorize and reflux at 80°C for 2 hours, then filter to remove activated carbon, then remove ethyl acetate to obtain decolorized and degreased pig gallbladder Paste 841g, this 841g crude bile paste is dissolved in the mass fraction of 4.2kg in the sodium hydroxide aqueous solution of 1%, the pH of adjustment solution is 8, uses the microfiltration membrane of 0.45 μm pore size, the ultrafiltration membrane of 0.01 μm pore size successively Remove suspended colloidal particle impurities by filtration to obtain clear components to be chromatographic...
Embodiment 2
[0036] Quantitatively weigh 1 kg of commercially available pig gall paste, put it in a 10-liter extraction tank, add 3.8 liters of cyclohexane and heat it to reflux at 80°C for 3 hours, remove the cyclohexane, and repeat this operation 2 more times to obtain degreased Crude gall paste 855g, this 855g thick gall paste is added 5L ethanol reflux dissolving, add 85g gac again after fully dissolving and take off reflux for 2 hours, filter and remove gac, then remove ethanol, obtain the decolorized degreasing thick gall paste 842g, this 842g rough Dissolve 4.2kg of 1% sodium hydroxide aqueous solution in the gall paste, adjust the pH of the solution to 9, and remove the suspended colloidal particle impurities by successively filtering with a microfiltration membrane with a pore size of 0.45 μm and an ultrafiltration membrane with a pore size of 0.01 μm Obtain clear components to be chromatographically separated;
[0037] Take an industrial chromatographic column with a column lengt...
Embodiment 3
[0039] Quantitatively weigh 1 kg of commercially available pig gall powder, put it in a 10-liter extraction tank, add 4.2 liters of n-hexane and heat it to reflux at 65°C for 3 hours, remove the n-hexane, and repeat this operation once more to obtain fat-free gallbladder Powder 845g, add 7.6L chloroform reflux and dissolve this 845g coarse gall powder, add 85g gac after fully dissolving and take off reflux for 2 hours, filter and remove gac, remove chloroform again, get decolorized degreasing coarse gall powder 831g, this 831g coarse gall powder Dissolve the powder in 4.2 kg of 1% sodium hydroxide aqueous solution, and then filter through a microfiltration membrane with a pore size of 0.45 μm and an ultrafiltration membrane with a pore size of 0.01 μm to remove the suspended colloidal particle impurities to obtain a clear component to be chromatographically separated ;
[0040] Take an industrial chromatographic column with a column length of 600 mm and an inner diameter of 13...
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