Novel method to prepare polystyrene-based monolithic columns for chromatographic and electrophoretic separations by microwave irradiation.
Novel method to prepare polystyrene-based monolithic columns for chromatographic and electrophoretic separations by microwave irradiation.
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DOI：
10.1016/j.chroma.2007.10.068
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发表时间：
2008-04
期刊：
影响因子：
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通讯作者：
Yu-Ping Zhang;X. Ye;Mengkui Tian;Ling‐bo Qu;Seong-Ho Choi;A. Gopalan;Kwang-Pil Lee
中科院分区：
文献类型：
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作者：
Yu-Ping Zhang;X. Ye;Mengkui Tian;Ling‐bo Qu;Seong-Ho Choi;A. Gopalan;Kwang-Pil Lee
微波辐照可以为整体毛细管柱的制备提供一种可行的替代方法，如紫外光和热引发。聚苯乙烯基整体固定相在熔融二氧化硅毛细管中原位制备，同时在小瓶中制备。采用压力辅助毛细管电色谱法（pCEC）、毛细管电色谱法（CEC）和低压液相色谱法（LPLC）评价柱的渗透性、电泳和色谱行为。采用最佳的单片材料，在pCEC模式下，用于制备硫脲柱的最大理论板可以接近18000个板/m。此外，用压汞孔隙法和扫描电镜系统地研究了致孔溶剂（甲苯/异辛烷）的组成对有机基单体[聚苯乙烯-二乙烯苯-甲基丙烯酸]形貌的影响。异辛烷含量高的单块体孔径大，渗透性好，分离速度快。
Microwave irradiation can provide a viable alternative to the traditional means such as ultraviolet light and thermal initiation for the preparation of monolithic capillary columns. Polystyrene-based monolithic stationary phases were prepared in situ in fused-silica capillaries and simultaneously in vials. The column permeability, electrophoretic and chromatographic behavior were evaluated using pressure-assisted capillary electrochromatography (pCEC), capillary electrochromatography (CEC) and low pressure liquid chromatography (LPLC). With an optimal monolithic material, the largest theoretical plates for preparing the column could be close to 18,000 plates/m for thiourea in the mode of pCEC. Furthermore, the influence of the composition of the porogenic solvents (toluene/isooctane) on the morphology of organic-based monoliths [poly(styrene-divinylbenzene-methacrylic acid)] was systematically studied with mercury intrusion porosimetry and scanning electron microscopy. The monoliths which were prepared with a high content of isooctane had a bigger pore size and better permeability, and hence resulted in a faster separation.