毛细管电色谱硅胶整体柱的制备与性能研究-有机化学专业毕业论文.docxVIP

南开大学2001级硕士研究生学位论文中文摘要 南开大学2001级硕士研究生学位论文 中文摘要 毛细管电色谱(CEC)是毛细管电泳(cE)和高效液相色谱(HPLC)的融合技术。它既 具有HPLC高选择性的优点，又具有CE高柱效、高分辨率、高选择性、快速、微量的优势。 毛细管电色谱作为一种新兴的微分离技术发展迅速，潜力巨大，是当今分析化学的研究热 点。然而一些涉及色谱柱和分离模式的实际困难，如气泡问题、色谱柱寿命短问题等大大 限制了毛细管电色谱的发展，使其尚不能作为有效的标准分析手段。目前专用制备色谱柱 的改进以及新型分离模式的研究已成为进～步开发电色谱潜力的关键，其中毛细管电色谱 整体柱的研究是公认有效解决上述困难的有效途径之一，也是当今电色谱研究的前沿课 题。 本论文采用热引发一步法制备毛细管电色谱硅胶整体柱。系统的研究并优化了制柱条 件，考察了单体比例、盐酸浓度、毛细管内径以及制柱反应时间等因素对柱制备的影响。 而且还通过使用表面活性剂或交联剂解决了均相的难题。本文在电色谱上评估了整体柱的 性能，深入探讨了有机溶剂比例、pH值、电压以及温度等电色谱操作条件对电渗流、保留 机理和柱效的影响。实现T9种苯的同系物和多环芳烃的基线分离；还基线分离了7种中性、 酸性和碱性物质。该柱柱效超过l 10，000plates／m。 关键词：毛细管电色谱，毛细管整体柱，硅胶整体柱 南开大学2001级硕士研究生学位论文Abstract 南开大学2001级硕士研究生学位论文 Abstract Capillary eletrochromatography(CEC)is a new miniaturized separation technique that combines the advantages of capillary electrophoresis(cE)and high performance liquid chromatograph fHPLC)．Due to high efficency,high selectivity,rapid separation and low consumption of both samples and solvents，CEC has received considerable attention in recent years and evolved as a promising analytical technique．However，there were still problems and difficulties associated with bubble formation and colunm dry-out in CEC．These problems can be addressed by capillary monolithic column．To data,this technique has been the most intersting 6eldinCEC． By optimizing preparation condition，we prepared different heat initiated silica monoliths by a one—step，in situ，process．Furthermore，using surfactant or cross—linker we overcame the problem of heterogeneous reactor and obtained the homogeneous reactor In addition，different parameters such as the volume of apply voltage，buffer pH，acetonitrile concentration and column temperature，were varied to assess their influence on retention mechanism，electroosmotic flow (EOF)and column efficiencies．Using this column a variety of polycyclic aromatic hydrocarbons were separated from mixture wim theoretical plate numbers greater than 1 1 0．000 plates／m． Keywords：Capillary eletrochromatography,Capillary monolithic column，Silica