Ye Fanggui, Xie Zenghong, Wu Xiaoping, Lin Xucong, Chen Guonan
The Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety, and Department of Chemistry, Fuzhou University, Fuzhou, Fujian 350002, China.
J Chromatogr A. 2006 Jun 9;1117(2):170-5. doi: 10.1016/j.chroma.2006.03.085. Epub 2006 Apr 18.
A novel stationary phase phenylaminopropyl silica (PhA-silica) monolith was successfully prepared for pressure assisted capillary electrochromatography (pCEC). The monolithic silica matrix from a sol-gel process was chemically modified by using [3-(phenylamino)propyl]trimethoxysilane as surface modification reagent to produce the phenylaminoporpyl function. The secondary amino groups on the surface of the monolithic stationary phase contributed to the generation of anodic electroosmotic flow (EOF) under acidic conditions. The phenyl group together with the spacer (-(CH(2))(3)-) in PhA-silica provides sufficient hydrophobic properties. To evaluate the column performance, effects of buffer pH and mobile phase composition on the mobile phase linear velocity and the retention factors of alkylbenzenes, phenols and anilines were investigated in pCEC mode. The monolithic stationary phases exhibit typical reversed-phase (RP) electrochromatographic behavior toward neutral solutes. Hydrophobic as well as electrophoretic migration process within the monoliths was observed for the separation of basic solutes such as anilines without peak tailing.
成功制备了一种用于压力辅助毛细管电色谱（pCEC）的新型固定相苯氨基丙基硅胶（PhA-硅胶）整体柱。采用溶胶-凝胶法制备的整体硅胶基质，以[3-(苯氨基)丙基]三甲氧基硅烷作为表面改性试剂进行化学改性，以产生苯氨基丙基官能团。整体固定相表面的仲氨基有助于在酸性条件下产生阳极电渗流（EOF）。PhA-硅胶中的苯基与间隔基（-(CH₂)₃-）一起提供了足够的疏水性能。为了评估柱性能，在pCEC模式下研究了缓冲液pH值和流动相组成对流动相线性速度以及烷基苯、酚类和苯胺类保留因子的影响。整体固定相对中性溶质表现出典型的反相（RP）电色谱行为。在分离苯胺等碱性溶质时，观察到整体柱内的疏水以及电泳迁移过程，且无峰拖尾现象。
