Preparation Of Organic Polymer-based Monolithic Column And Its Applications In Capillary Electrochromatography

In recent years, capillary monolithic columns, as the separation media of thefourth generation, have attracted considerable attention due to their unique propertiessuch as the ease of their preparation, good permeability and high stability. Amongthem, organic polymer-based monolithic columns have been widely applied. Theyprovide a wide pH range, good bio-compatibility and facile chemical modifications.The available monomers are also various in their preparation. Neverthless, thedrawbacks of organic polymer-based monolith are hetergeneous structure, relativelylow column efficiency and commercialization. To solve these problems, it is of greattheoretical and practical significances to improve the fabrication of CEC monolithiccolumns, develop new preparation techniques and extend their applications.The contents of this thesis are composed of four parts as follows.In chapter1, the brief history and principle of CEC, the development of CECmonolith technologies and their applications were reviewed. The significance andcontents of this research were also introduced,In chapter2, a lauryl methacrylate-based CEC monolithic column waspreparated via a free radical polymerization and then evaluated. Three β2-agonistswere rapidly separated within4min by CEC using this monolith. With thecombination of on-line concentration technique, the concentration factors of45-fold,36-fold and320-fold were obtained for salbutamol, procaterol and formoterolcompared to normal injection, respectively. The proposed method was successfullyapplied to the determination of salbutamol in human urine.In chapter3, a novel stearyl methacrylate-based CEC monolithic column waspreparated via high intenal phase emulsion (HIPE) templating and then evaluated.Compared with conventional CEC monolith, the polyHIPE monolith showed somemerits of well-defined macropores, excellent permeability and high stablity.Furthermore, EOF generation came from sulfate groups of the initiator. Theseproperties met the requirement of high-efficiency and rapid separation. Five dopingwere rapidly separated within7min by CEC using this polyHIPE monolithic column. In chapter4, a microemulsion electrokinetic capillary chromatography methodwas developed for the rapid analysis of six plant hormones. Microemulsioncomposition were systematically studied and parameters of large volumn sample stackon-line concentration technique were optimized. Under optimized conditions, sixplant hormones were rapidly separated within10min. The detection limits (S/N=3)were0.04,0.05,0.05,0.04,0.05and0.05μg/mL for abscisic acid, indole-3-butyricacid, indole-3-acetic acid,1-naphthylacetic acid, indole-3-propionic acid and salicylicacid, respectively. The proposed method was simple, rapid, sensitive and could beapplied to the determination of six plant hormones in spiked water and1-naphthylacetic acid in leaf fertilizer.