Chiral Separation of Chlorpheniramine by Capillary Electrophoresis *L

Aim To study the chiral separation of chlorpheniramine(Chp) by using a mixture of β CD and glutamate β CD as the chiral additive in CE. Methods Mixture of β cyclodextrin and glutamate β cyclodextrin was used as a chiral selector to the separation of chlorpheniramine. The effects of the concentrations of β cyclodextrin and glutamate β cyclodextrin, the voltage and the pH of buffers on the separation of chlorpheniramine were studied. Results The chiral recognization of the mixed chiral selector was better than that of a single selector. At pH below 4, the pH of buffers did not affect the separation and the separation of chlorpheniramine had good reproducibility. Conclusion Using a mixture of β CD and Glu β CD as chiral selector is useful for the enantioseparation of Chp in CE.

Enantiomeric separation of phenylsuccinic acid by cyclodextrin-modified reversed phase high-performance liquid chromatography

The chiral separation of phenylsuccinic acid(PSA)was studied by reversed phase high-performance liquid chromatography(RP-HPLC)with cyclodextrins(CDs)as chiral mobile phase additives.The effects of types of CDs,concentration of hydroxypropyl-β-cyclodextrin(HP-β-CD),percentage of organic modifier,pH value and column temperature on enantioselective separation were investigated.The quantification property of the developed RP-HPLC method was examined.The chiral recognition mechanism of PSA was also discussed.The results show that a baseline separation of PSA enantiomers is achieved on a Lichrospher C18 column(4.6 mm(inner diameter)×250 mm,5μm)with HP-β-CD as chiral mobile phase additive.The capacity factors of R-PSA and S-PSA are 3.94 and 4.80,respectively.The separation factor and resolution are respectively 1.22 and 8.03.The mobile phase is a mixture of acetonitrile and deionized water(20-80,volume ratio)containing 10 mmol/L HP-β-CD and 0.05% trifluoroacetic acid(pH 2.5,adjusted with triethylamine)with a flow rate of 1.0 mL/min.The ultraviolet(UV)detector is set at 254 nm.The likely roles are inclusion interaction,induction and hydrogen bonding between HP-β-CD and PSA enantiomers.

盐酸舍曲林的手性分离与纯度检查

目的:建立手性分离盐酸舍曲林的毛细管区带电泳方法,并检查光学纯度。方法:采用未涂层石英毛细管(50 cm×50μm,有效长度40 cm),考察了手性选择剂的种类、浓度,缓冲液种类、pH、分离电压对手性拆分的影响,从而确定最佳分离条件。结果:盐酸舍曲林对映异构体的分离电泳条件为:以25 mmol·L-1磷酸-三乙醇胺(pH为2.50,内含3%β-环糊精硫酸钠盐)为运行缓冲液;检测波长为214 nm;工作电压为-20 kV,温度为25℃。结论:该毛细管电泳法能基线分离盐酸舍曲林的4个异构体;能有效检查盐酸舍曲林的光学纯度,该方法可用于该原料及其相关制剂的异构体杂质的质量控制和稳定性研究。

毛细管电泳手性拆分西他沙星异构体

目的:建立西他沙星及其异构体高效毛细管电泳拆分的新方法。方法:以β-环糊精及几种环糊精衍生物作为手性添加剂,采用毛细管电泳分离新型抗菌素西他沙星与其3个异构体。对运行缓冲液的浓度、pH,环糊精的种类、二元环糊精体系中环糊精的比例,分离电压,柱温,有机改性剂等因素对分离的影响进行考察,并对拆分机制进行初步探讨。结果:运行缓冲液为含2%硫酸化-β-环糊精和1%β-环糊精的25 mmol.L-1的磷酸二氢钾-磷酸缓冲溶液(pH 2.5),操作电压为-25kV,柱温为25℃,检测波长为295 nm,西他沙星与其3个异构体达到良好分离。结论:所建立的毛细管电泳方法简便,适用于西他沙星异构体的检查。