高效液相色谱手性流动相添加剂法拆分氯噻酮对映体

Resolution of chlorthalidone enantiomers by high performance liquid chromatography with chiral mobile phase additive

应用反向高效液相色谱,以羟丙基-β-环糊精(HP--βCD)作为手性流动相添加剂,拆分了氯噻酮(Chlorthalidone)对映体。对主要的影响因素如羟丙基-β-环糊精浓度、流动相pH值、三乙胺(TEA)、甲醇、柱温、流速等进行了系统研究,建立了羟丙基-β-环糊精流动相添加剂法拆分氯噻酮对映体的方法。使用HarbonLichrospher-C18色谱柱(5μm,150 mm×4.6 mm),流动相为V(甲醇)∶V(水相)=20∶80(水相含30 mmol/L HP--βCD0、.1 mol/L Na2HPO4、体积分数2%的TEA、pH5),流速为0.8 mL/min,室温下拆分,氯噻酮对映体可得到良好分离。

Chlorthalidone enantiomers were separated by reversed phase high performance liquid Chromatography using hydroxypropyl-β-cyclodextrin as a chiral mobile phase additive. The main influence such as concentration of hydroxypropyl-β-cyclodextrin, pH of mobile phase, TEA additive, methanol, temperature of column, flow rate were investigated systematically, and the method of resolution of Chlorthalidone enantiomers using hydroxypropyl-β-cyclodextrin as the chiral mobile phase additive was set up. The results showed that nearly baseline separation was obtained when Harbon Lichrospher-C18 chromatography column（5μm, 150 mm×4.6mm） was used, and the mobile phase was composed of methanol ： aqueous phase = 20 ： 80 （aqueous phase was composed of 30 mmol/L HP-β-CD, 0. 1 mol/L Na2HPO4, 2%TEA, pH 5）, at the flow rate of 0.8 mL/min, being resolved under the ambient temperature.