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目的 :研究适用于毛细管电色谱乃至液相色谱的具有可定制选择性的固定相 ,以便利用这些新型的固定相 ,对于难以采用常规的固定相分离的物质实现选择性的分离。方法 :将商品球形硅胶颗粒 (粒径 5 μm)与乙烯基三乙氧基硅烷通过在无水甲苯中回流 1 8h ,进行硅烷化修饰。在硅烷化了的硅胶颗粒上 ,通过偶氮异丁腈作为引发剂 ,在正己醇和乙腈 (1∶4 )的混合溶剂中 ,80℃下反应 1 8h ,引发苯乙烯 二乙烯基苯的链式聚合反应 ,以及苯乙烯 二乙烯基苯共聚物通过硅胶表面上的乙烯基键合到硅胶表面上的键合反应。所得到的包覆了这种高聚物的硅胶颗粒 (PS DES)本身也是一种非传统的毛细管电色谱用的固定相。所产生的PS DES再和氯磺酸发生磺化反应 ,即得到磺酸型的强阳离子交换型固定相。结果 :将所制得的PS DES固定相以及磺化的固定相各自填充到毛细管内 ,考察这些毛细管电色谱柱的色谱性能 ,发现前者表现出反相固定相的性质。由于所包覆高聚物中的苯基基团 ,这种固定相在色谱分离过程中引入了π -π电子相互作用 ,因此对芳香化合物表现出了独特的选择性 ,在其上成功地分析了一些芳香化合物以及极性的和碱性的药物。在磺酸型的固定相上 ,则成功地分离了一些碱性药物 ,得到了较好的对称峰型 ,这些药物间可达到基线分
OBJECTIVE: To study the customizable, selective stationary phases for capillary electrochromatography and even liquid chromatography in order to exploit these novel stationary phases for the selective separation of substances which are difficult to remove by conventional stationary phases. Methods: The spherical silica particles (particle size 5 μm) and vinyl triethoxysilane were refluxed in anhydrous toluene for 18 h for silanization. On the silylated silica gel particles, azo isobutyronitrile was used as the initiator to react for 18 h at 80 ℃ in a mixed solvent of n-hexanol and acetonitrile (1: 4) to initiate the reaction of styrene-divinylbenzene The polymerization reaction, as well as the bonding reaction of the styrene divinylbenzene copolymer onto the surface of the silica gel through the vinyl group on the surface of the silica gel. The resulting PS DES coated with such a polymer itself is also a non-traditional stationary phase for capillary electrochromatography. The resulting PS DES sulfonated with chlorosulfonic acid and then sulfonated to give a strong cation-exchange stationary phase. Results: The prepared PS DES stationary phase and the sulfonated stationary phase were filled into the capillary respectively. The chromatographic properties of these capillary column were investigated. The former showed the properties of reversed-phase stationary phase. Due to the phenyl groups in the polymer to be coated, this stationary phase introduces π-π electron interactions during the chromatographic separation and thus exhibits a unique selectivity for aromatic compounds on which successful analysis Some aromatic compounds as well as polar and basic drugs. On the sulfonic stationary phase, some basic drugs were successfully separated and a good symmetrical peak pattern was obtained, with a baseline score of these drugs