新型直链淀粉手性固定相拆分戊唑醇对映体

采用新型直链淀粉-三(5-氯-2-甲基苯基氨基甲酸酯)涂敷型手性固定相在反相色谱条件下拆分戊唑醇对映体,评价了流动相组成(甲醇/水,乙腈/水)及柱温(5～45℃)对对映体分离的影响。结果表明：以甲醇/水为流动相时,在甲醇含量100%至40%范围内,戊唑醇对映体均无分离趋势；而用乙腈/水为流动相时,在乙腈含量100%至40%范围内,戊唑醇对映体均可实现基线分离；在5～45℃,V(乙腈)∶V(水)=1∶1,对映体的保留因子(k)与分离因子(α)随温度升高而降低,分离度(RS)却先升后降,基于线性Van't Hoff曲线的热力学参数证明戊唑醇对映体的分离受焓驱动。

Enantiomeric separation of tebuconazole by new type of amylose chiral stationary phase

The separation of tebuconazole enantiomers was performed by high-performance liquid chromatography (HPLC) on the amylose-tris (5-chlorine-dimethy-phenylcarbamate) chiral stationary phase using reverse phase mode. The effects of different mobile phase compositions (methanol/water, acetonitrile/water) and column temperature (5-45℃) on the chiral separation were investigated. The results showed that tebuconazole enantiomers did not separate using methanol/water as mobile phase with the content of methanol ranging from 100% to 40%. In contrast, baseline separation of enantiomers was achieved using acetonitrile/water as mobile phase with the content of acetonitrile ranging from 100% to 40%. The retention factors (k) and selectivity factor (α) decreased when the temperature increased from 5℃ to 45℃, while the resolution (RS) of enantiomers first increased and then decreased within the same range of temperature (acetonitrile/water,50/50, V/V). Thermodynamical parameters illustrated that separation of tebuconazole enantiomers was driven by enthalpy.