Yan Lijuan, Zhang Qinghe, Zhang Weibing, Feng Yuqi, Zhang Lihua, Li Tong, Zhang Yukui
Department of Chemistry, Wuhan University, China.
Electrophoresis. 2005 Aug;26(15):2935-41. doi: 10.1002/elps.200500016.
A novel hybrid organic-inorganic silica-based monolithic column possessing phenyl ligands for reversed-phase (RP) capillary electrochromatography (CEC) is described. The monolithic stationary phase was prepared by in situ co-condensation of tetraethoxysilane (TEOS) with phenyltriethoxysilane (PTES) via a two-step catalytic sol-gel procedure to introduce phenyl groups distributed throughout the silica matrix for chromatographic interaction. The hydrolysis and condensation reactions of precursors were chemically controlled through pH variation by adding hydrochloric acid and dodecylamine, respectively. The structural property of the monolithic column can be easily tailored through adjusting the composition of starting sol solution. The effect of PTES/TEOS ratios on the morphology of the created stationary phases was investigated. A variety of neutral and basic analytes were used to evaluate the column performance. The CEC columns exhibited typical RP chromatographic retention mechanism for neutral compounds and had improved peak shape for basic solutes.
描述了一种新型的具有苯基配体的有机-无机杂化硅胶整体柱，用于反相（RP）毛细管电色谱（CEC）。整体固定相通过四乙氧基硅烷（TEOS）与苯基三乙氧基硅烷（PTES）的原位共缩合，经由两步催化溶胶-凝胶法制备，以引入分布在整个硅胶基质中的苯基用于色谱相互作用。分别通过添加盐酸和十二烷基胺，通过pH变化对前体的水解和缩合反应进行化学控制。通过调整起始溶胶溶液的组成，可以轻松调整整体柱的结构性质。研究了PTES/TEOS比例对所制备固定相形态的影响。使用多种中性和碱性分析物评估柱性能。CEC柱对中性化合物表现出典型的反相色谱保留机制，对碱性溶质具有改善的峰形。
