串联色谱分离床层的制备及表征

Preparation and characterization of the tandem separation beddings

制备了一种由甲基丙烯酸酯整体床层和C18反向色谱填料串联的微径色谱柱.从串联柱各部分的扫描电镜图可看出:毛细管柱前端形成了多孔网络骨架结构,整体床层部分与毛细管内壁结合紧密,同时后段部分C18填料填充均匀.采用自组装的微流液相系统对其进行了色谱评价,实现了四种模型化合物的基线分离.随着整体床层长度的逐渐减少,未见色谱柱效明显变化,且经过数百次的色谱平衡、冲洗及分离后,分离床层结构仍然十分稳定.

A tandem micro-column was prepared,which consisted of the forepart polymethacrylate-based monolith and the reverse phase packing material of C18.A scanning electron micrograph of different cross-sections of the prepared column showed that the morphologies of the dual stationary phases detailedly.It could be seen that a porous network was formed in the center of the capillary and adhered to the column inner wall in the monolithic section,moreover,a slurry packing of C18 was homogenously obtained in the packing section.The self-assembled capillary liquid chromatographic system was used to evaluate its chromatographic performance,with the baseline separation of four model analytes.With the change of the monolithic length,no apparent change of column efficiency was observed throughout the experiments,and stable bedding structures could still be remained after several hundreds of chromatographic equilibrium,flush and separation.