金纳米粒子修饰毛细管硅胶整体柱的制备及其电色谱性能研究  

Preparation and Characterization of Gold Nanoparticle-Modified Silica Monolith for Capillary Electrochromatography

作　　者：叶芳贵[1] 陆俊宇[1] 王圆[1] 张爱珠[1] 田建袅[1] 赵书林[1] 

机构地区：[1]广西师范大学化学化工学院,药用资源化学与药物分子工程教育部重点实验室,桂林541004

出　　处：《分析化学》2011年第3期341-345,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21065002);广西师范大学药用资源化学与药物分子工程教育部重点实验室主任基金(No.07109001-08)资助

摘　　要：通过毛细管硅胶整体柱表面修饰十八烷基硫醇金纳米粒子,制备了一种新型毛细管电色谱固定相。制备金纳米粒子修饰整体柱时,采用溶胶-凝胶法制备毛细管硅胶整体柱,并在其表面化学修饰3-巯基丙基三甲氧基硅烷;通过巯基基团固载金纳米粒子于整体柱上,再共价键合十八烷基硫醇于金纳米粒子表面。以甲苯为探针,对理论塔板高度与流动相线速度之间的关系进行了考察,其最小理论塔板高度约为7.8 mm。考察了操作条件如流动相中的有机改性剂和缓冲溶液pH值对金纳米粒子修饰毛细管整体柱电渗流的影响,并与相应的毛细管硅胶整体柱(Silica)进行比较。以烷基苯同系物为模型化合物,评价了Silica、巯基(Silica-SH)和十八烷基(Silica-GNPs-C18)3种整体柱电色谱性能;还考察了烷基苯同系物在Silica-GNPs-C18上的保留行为。结果表明,其保留机理是基于典型的反相作用。另外,在甲醇含量为15%的流动相条件下,Silica-GNPs-C18还可实现4种极性苯酚类物质的基线分离。A novel silica monolithic stationary phase functionalized with octadeeanethiol gold nanoparticles was prepared for capillary electrochromatography （CEC）. The bare monolithic silica column was prepared by a sol-gel process and has been chemically modified with 3-mercaptopropyl-trimethoxysilane, followed by immobilization of gold nanoparticles and modification by octadecanethiol. The relationship between plot of plate height and the linear velocity on gold nanoparticle-modified silica monolith was investigated, and a minimum plate height of about 7.8 gm for toluene was obtained. The electroosmotic flow characteristics of the gold nanoparticle-modified silica monolith and bare silica monolith （Silica） were studied by varying the percentage of organic modifier in buffer and buffer pH. To evaluate the column performance, hydrophobic alkylbenzenes as model compounds were tested on the prepared Silica, SH-modified （Silica-SH） and octadecanethiol modified （Silica-GNPs-C18） monoliths. The electroehromatographic retention behavior of alkylbenzenes on Silica-GNPs-C18 column was also investigated. The experiment results showed that Silica-GNPs-C18 column exhibits typical reversed phase electrochromatographic behavior toward neutral solutes. Reversed phase CEC separations of four selected polar phenols were also demonstrated on Silica-GNPs-C18 column using mobile phase containing 15% methanol.

关 键 词：金纳米粒子 毛细管电色谱 硅胶整体柱 溶胶-凝胶 

分 类 号：O657.7[理学—分析化学]