Separation And Purification Of Ursodeoxycholic Acid

Ursodeoxycholic acid was separated and purified from the product of electro-reduction through macroporous resin method,silanization method and alkaline ion exchange resin method,respectively.When macroporous resin method was used to separate and purify ursodeoxycholic acid,HZ-802 resin was chosen as the separation medium.The adsorption capacity of resin HZ-802 to ursodeoxycholic acid was as high as 90.7 mg/mL wet resin.The optimal conditions were:sample concentration was 100 mg/mL,height-diameter ratio was 30:1,90%methanol was as eluent at 0.8 mL/min,pH was 7.0.The recovery of ursodeoxycholic acid was 78.4%and the purity was 94.7%.When silanization method was used to separate and purify ursodeoxycholic acid,the N,N-dimethylformaminde was used as solvent,hexamethyldisilazane as the silylating agent.At 60?,the ratio of raw crude ursodeoxycholic acid,N,N-dimethylformamide and hexamethyldisilazane was 1:10:2(w/v/v),2 h after the reaction,the recovery and purity of ursodeoxycholic acid were 99.8%and 99.5%,respectively.When alkaline ion exchange resin method was used to separate and purify ursodeoxycholic acid,D201 resin was chosen as the separation medium.The results implied the Langmuir isotherm equation can describe the adsorption process of ursodeoxycholic acid on D201 resin.At 25?,the sample concentration was 10 mg/mL,gradient elution was conducted with 0.05 M NaCl and 0.1 M NaCl at 1.0 mL/min.Final ursodeoxycholic acid recovery was 76.7%,with a purity of 83.2%.