色谱

色谱

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毛细管硅胶基质整体柱的制备及其电色谱性能研究

邵华1,邓启良1,伦志红1,阎超2,高如瑜1   

  1. 1. State Key Laboratory of Elemento-Organic Chemistry, Institute of Elemento-Organic Chemistry, Nankai University, Tianjin 300071, China; 2. Unimicro Technologies Co., Ltd., Shanghai 201203, China
  • 收稿日期:2004-05-17 修回日期:1900-01-01 出版日期:2005-05-30 发布日期:1988-09-25
  • 通讯作者: 高如瑜
  • 基金资助:

Preparation and Evaluation of Monolithic Silica Columns for Capillary Electrochromatography

SHAO Hua1, DENG Qiliang1, LUN Zhihong1, YAN Chao2, GAO Ruyu1   

  1. 1. State Key Laboratory of Elemento-Organic Chemistry, Institute of Elemento-Organic Chemistry, Nankai University, Tianjin 300071, China; 2. Unimicro Technologies Co., Ltd., Shanghai 201203, China
  • Received:2004-05-17 Revised:1900-01-01 Online:2005-05-30 Published:1988-09-25

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摘要： 采用热引发一步法制备了毛细管电色谱硅胶基质整体柱。通过使用表面活性剂(十二烷基磺酸钠)增加了反应液中两相之间的相互溶解,使得反应液最终成为均相溶液,实现了硅胶整体柱的均相聚合制备。所制备的均相硅胶整体柱内部结构更加均匀,大大提高了分离度。评价了该整体柱的电色谱性能,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。在该均相硅胶基质整体柱上成功地分离了9种中性物质(硫脲、苯、甲苯、乙基苯、正丙苯、萘、正丁基苯、芴和蒽)以及7种中性、酸性和碱性物质(硫脲、邻氨基酚、苯酚、苯、邻甲苯胺、α-萘胺和2,4-二氯苯胺)。该柱对硫脲的柱效超过110000塔板/m。

关键词: 硅胶基质整体柱, 毛细管电色谱, 毛细管整体柱, 制备

Abstract: A solution of methacryloxypropyltrimethoxysilane in the presence of an acid catalyst, water, toluene and azobisisobutyronitrile (AIBN) was initiated at 60 ℃ for 24 h in a 100 μm i.d. capillary to prepare a porous monolithic silica column by a one-step, in situ, process. Various parameters, such as the volume of applied voltage, buffer pH, acetonitrile concentration and column temperature, were varied to assess their influence on retention mechanism, electroosmotic flow (EOF) and column efficiencies. The heat initiated sol-gel capillary monolithic column showed reversed-phase behavior. Furthermore, the homogeneous reactor was obtained using surfactant (sodium dodecyl sulfate, SDS). The baseline separation of 9 neutral compounds (thiourea, benzene, toluene, ethyl benzene, n-propylbenzene, naphthalene, n-butylbenzene, fluorene and anthracene) and 7 acidic, basic and neutral compounds (thiourea, o-aminophenol, phenol, benzene, o-methylaniline, α-naphthylamine, 2,4-dichloroaniline) can be obtained under optimized capillary electrochromatographic conditions. Column efficiency of 110000 plates/m was achieved for thiourea.

Key words: capillary monolithic column, monolithic silica columns, preparation , capillary eletrochromatography