二维毛细管区带电泳/胶束电动毛细管色谱分离尿样中的药物及其对映体

建立了毛细管区带电泳(CZE)/胶束电动毛细管色谱(MEKC)二维毛细管电泳分离平台,CZE毛细管和MEKC毛细管通过一段带微孔的聚四氟乙烯(polytetrafluoroethylene,PTFE)套管固定。样品在CZE毛细管中分离后进入MEKC毛细管进一步分离,在二维转换过程中采用动态pH连接-胶束扫集法避免第一维分离区带在接口处扩散。将该方法成功用于鼠尿样品中4种药物及其对映体的分离,各组分的理论塔板数为(2.8～4.3)×104/m,检出限为0.015～0.052mg/L,实际样品中峰面积和迁移时间的相对标准偏差(n=7)分别为1.7%～3.8%和1.3%～4.6%。方法重现性好、灵敏度和分离度高、峰容量大,适用于尿样中多种药物组分及其对映体的同时分离检测。

Two dimensional capillary zone electrophoresis/micellar electrokinetic capillary chromatography for the analysis of drugs and their enantiomers in urine samples

A new two dimensional method, which interfaced capillary zone electrophoresis (CZE) and micellar electrokinetic capillary chromatography (MEKC) by a polytetrafluoroethylene (PTFE) tube with a hole of 30~40 μm diameter on the top, was developed for the analysis of drugs and their enantiomers. The CZE was used as the first dimensional separation, from which the eluting components were transferred and further analyzed by MEKC. Online dual concentration method, pH junction-sweeping, was used to avoid sample zone diffusion at the interface. The separation efficiencies and detection limits were (2.8~4.3)×104/m and 0.015~0.052 mg/L, respectively. The proposed method has successfully demonstrated that in the separation of four drugs and their enantiomers in urine samples, the relative standard deviations (RSDs) of peak area and migration time were in the ranges of 1.7%~3.8% and 1.3%~4.6%, respectively. The method was proved to have good reproducibility, high sensitivity and resolution, large peak capacity. It is reliable and suitable to separate and determine multi-drugs and their enantiomers in urine samples simultaneously.