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机构地区:[1]岛科技大学化学与分子工程学院,生态化工教育部重点实验室,青岛266042 [2]青岛理工大学理学院,青岛266033
出 处:《中国科学:化学》2010年第5期523-530,共8页SCIENTIA SINICA Chimica
基 金:国家自然科学基金项目(20775039)资助
摘 要:将在线富集技术同二维(2D)毛细管电泳(CE)分离相结合同时提高复杂样品中痕量组分的分离度和检测灵敏度.毛细管区带电泳(CZE)作为第一维,分析物根据淌度不同进行分离,第一维流出组分进入第二维毛细管,根据分配系数不同进行胶束电动毛细管色谱(MEKC)分离.采用阳离子选择性耗尽进样(CSEI)在柱预富集,延长进样时间,增大进样量;同时在二维毛细管接口处采用动态pH联接/胶束扫集在线富集技术不仅避免第一维分离组分在接口处扩散,还可进一步压缩样品区带.同常规电动进样CE分离相比,该在线富集二维分离技术的分离能力远远高于一维CZE或MEKC分离,富集倍数达到(0.5~1.2)×104.该法成功应用于人体尿样中四种药物及对映体的分析测定,浓度检出限为0.1~0.3μg/L.进一步研究了人体尿样中四种药物24h内的药代动力学规律.A novel method has been developed by integration of multi-concentration and two-dimensional (2D) capillary electrophoresis (CE) for simultaneous enhancement of detection sensitivity and separation power in complex samples.Capillary zone electrophoresis (CZE) was used as the first dimension separation according to mobilities,from which the effluent fractions were further analyzed by micellar electrokinetic capillary chromatography (MEKC) acting as the second dimension.Cation-selective exhaustive injection (CSEI) preconcentration method was used to introduce more analytes into the capillary.Furthermore,pH junction and sweeping dual concentration strategies were employed to avoid sample zone diffusion at the interface.The resulting electrophoregram was quite different from that of either CZE or MEKC separation.Up to (0.5-1.2)×104 fold improvements in sensitivity were obtained relative to conventional electrokinetic injection method.The proposed method was successfully applied to the determination of drugs in human urine.
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