CAS Key Laboratory of Separation Science for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China.
Anal Chim Acta. 2013 Jan 25;761:209-16. doi: 10.1016/j.aca.2012.11.052. Epub 2012 Dec 5.
A simple approach to fabricate hybrid monolithic column within the confines of fused-silica capillaries (75 μm i.d.) was introduced. A polyhedral oligomeric silsesquioxanes (POSS) reagent containing a methacrylate group was selected as functional monomer, and copolymerized with bisphenol A dimethacrylate (BPADMA) or ethylene dimethacrylate (EDMA) in the presence of porogenic solvents via thermally initiated free radical polymerization. After optimization of the preparation conditions, two POSS-containing hybrid monoliths were successfully prepared and exhibited good permeability and stability. By comparison of the separation efficiencies of the resulting poly(POSS-co-BPADMA) and poly(POSS-co-EDMA) monoliths in capillary electrochromatography (CEC) and capillary liquid chromatography (cLC), it was indicated the former has better column efficiencies for alkylbenzenes, phenols, anilines and PAHs in CEC and cLC than the latter. Particularly, the hybrid poly(POSS-co-BPADMA) monolith is more suitable for separation of PAHs due to π-π interaction between the analytes and aromatic rings in the surface of monolithic stationary phase.
介绍了一种在熔融石英毛细管（75μm ID）范围内制造混合整体柱的简单方法。选择了一种含有甲基丙烯酰基的多面体低聚倍半硅氧烷（POSS）试剂作为功能单体，并在致孔溶剂的存在下，通过热引发自由基聚合与双酚 A 二甲基丙烯酸酯（BPADMA）或乙二醇二甲基丙烯酸酯（EDMA）共聚。在优化制备条件后，成功制备了两种含有 POSS 的混合整体柱，表现出良好的渗透性和稳定性。通过比较所得聚（POSS-co-BPADMA）和聚（POSS-co-EDMA）整体柱在胶束电动色谱（CEC）和毛细管液相色谱（cLC）中的分离效率，表明前者在 CEC 和 cLC 中对烷基苯、酚、苯胺和多环芳烃具有更好的柱效，而后者则具有更好的柱效。特别是，由于分析物与整体固定相表面的芳环之间存在π-π相互作用，混合聚（POSS-co-BPADMA）整体柱更适合分离多环芳烃。
