Enantioseparation of aminoglutethimide was performed by high-speed counter-current chromatography with a two-phase system composed of ethyl acetate: methanol: water = 10: 1: 9. The lower phase contained 20 mmol/L ...Enantioseparation of aminoglutethimide was performed by high-speed counter-current chromatography with a two-phase system composed of ethyl acetate: methanol: water = 10: 1: 9. The lower phase contained 20 mmol/L of carboxymethly-β-cyclodextrin as chiral selector. The enantiomers were separated in 1.2 h and identified by chiral HPLC. This method was very efficient for the chiral preparative separation.展开更多
Objective To develop an efficient method for separating and purifying puerarin from the roots of Pueraria lobata.Methods Separation by fast centrifugal partition chromatography(FCPC)was processed with a biphasic sol...Objective To develop an efficient method for separating and purifying puerarin from the roots of Pueraria lobata.Methods Separation by fast centrifugal partition chromatography(FCPC)was processed with a biphasic solvent system composed of ethyl acetate-n-butanol-water(2:1:3).The separation conditions were determined as follows:sample loading of 10 mg,flow rate of 2 mL/min,rotation speed of 2200 r/min,ascending mode,and detection wavelength of 254 nm.High speed countercurrent chromatography(HSCCC)was used as a comparative method with the rotation speed of 800 r/min,flow rate of 2.0 mL/min,and sample loading of 10 mg in tail-to-head mode.Results Puerarin was obtained by FCPC with a resolution of 0.90 and a purity above 99%,while a resolution below 0.50 and a purity below 90%by HSCCC.Compared with HSCCC,FCPC has the advantages with higher purity and better resolution.Conclusion FCPC is a powerful method to separate and purify puerarin.展开更多
基金The work is supported by National Natural Science Foundation of China (No. 30160092) TRAP0YT and Yunnan Province's Natural Science Foundation.
文摘Enantioseparation of aminoglutethimide was performed by high-speed counter-current chromatography with a two-phase system composed of ethyl acetate: methanol: water = 10: 1: 9. The lower phase contained 20 mmol/L of carboxymethly-β-cyclodextrin as chiral selector. The enantiomers were separated in 1.2 h and identified by chiral HPLC. This method was very efficient for the chiral preparative separation.
基金International Science and Technology cooperation project of Shanghai(No.12120701400,2012)
文摘Objective To develop an efficient method for separating and purifying puerarin from the roots of Pueraria lobata.Methods Separation by fast centrifugal partition chromatography(FCPC)was processed with a biphasic solvent system composed of ethyl acetate-n-butanol-water(2:1:3).The separation conditions were determined as follows:sample loading of 10 mg,flow rate of 2 mL/min,rotation speed of 2200 r/min,ascending mode,and detection wavelength of 254 nm.High speed countercurrent chromatography(HSCCC)was used as a comparative method with the rotation speed of 800 r/min,flow rate of 2.0 mL/min,and sample loading of 10 mg in tail-to-head mode.Results Puerarin was obtained by FCPC with a resolution of 0.90 and a purity above 99%,while a resolution below 0.50 and a purity below 90%by HSCCC.Compared with HSCCC,FCPC has the advantages with higher purity and better resolution.Conclusion FCPC is a powerful method to separate and purify puerarin.