【作者】 付红靖；

【导师】 邹汉法；

【作者基本信息】 中国科学院研究生院（大连化学物理研究所） ， 分析化学， 2004， 博士

【摘要】 毛细管电色谱是近年来新兴的高效、快速的微分离分析技术，是色谱领域的研究热点之一。目前，毛细管电色谱的研究主要集中在毛细管电色谱柱的制备技术和毛细管电色谱的应用两个方面。 针对极性化合物分离困难的问题，提出了亲水作用电色谱的分离模式。在亲水作用电色谱的模式下成功地分离了小肽、吡啶等极性化合物，并对可能的保留机理进行了探讨。在亲水作用电色谱的模式下对碱性药物的保留行为进行了考察，建立了亲水作用毛细管电色谱定量分析血清中碱性药物的方法。 采用原位聚合的方法制备出强阴离子交换／反相混合模式毛细管电色谱整体柱。由于这种整体柱带有正电荷，避免了碱性化合物与固定相之间的静电吸引作用，从而避免碱性化合物的峰拖尾或不出峰等现象。建立了苯胺、碱性药物在强阴离子交换／反相混合模式下的毛细管电色谱分离方法。 制备了两性电荷型毛细管整体柱。该毛细管电色谱整体柱电渗流的大小和方向可以方便地通过改变流动相的pH值来调控。在同一根毛细管整体柱上，使用不同pH值的流动相可以使得化合物在不同的分离模式下进行分离，从而获得不同的选择性。 合成了L-谷氨酰胺改性脲醛树脂毛细管整体柱，在配体交换电色谱的模式下对氨基酸进行了手性分离。这是脲醛树脂作为电色谱整体柱材料的首次报道。更多还原

【Abstract】 Capillary electrochromatography (CEC) has been considered as a very promising analytical technique that combines the efficiency of capillary zone electrophoresis and the selectivity of liquid chromatography with the use of stationary phases. At present, research works on CEC are mainly focused on both the preparation of columns and its application.CEC separation mode with hydrophilic interaction stationary phases has been established for separation of polar compounds. The retention mechanisms were also systematically investigated, and it was observed that the retention factors of the tested compounds are increased with their polarity. Several types of polar compounds such as peptides, pyridines and basic Pharmaceuticals have been well separated. Furthermore, a method using hydrophilic interaction CEC is also developed for the determination of basic Pharmaceuticals spiked in human serum.CEC separations with mixed-modes of reversed-phase and aniqn-exchange stationary phases was proposed in the capillary monolithic column, which was prepared by in-situ polymerization of 2-(methacryloxy)ethyltrimethylammonium methyl sulfate (MEAMS) and ethylene dimethacrylate (EDMA) in the presence of porogens. The ammonium groups on the surface of the Stationary phase generate an electroosmatic flow (EOF) from cathode to anode, and serve as a strong anion-exchange stationary phase at the same time. Separations of aromatic compounds and basic compounds on the prepared column were performed under the mode of CEC.A zwitterionic monolithic column was prepared for CEC by in-situpolymerization of 2-(dimethyl amino)ethyl methacrylate (DMAM), methacrylic acid (MAA), butyl methacrylate (BMA) and ethylene dimethacrylate (EDMA). So there are two kinds of ionic groups, i.e., amino group and carboxyl group, on the surface of the staionary phase, and the EOF on the prepared column can be easily controlled by changing pH of the mobile phase, and several types of compounds have been successfully separated.A new type of monolithic CEC column based on the urea-formaldehyde resin was prepared, chiral separation of amino acids was achieved by using ligand-exchange interaction under the mode of CEC.更多还原