Qu Qi-Shu, Wang Song, Mangelings Debby, Wang Cheng-Yin, Yang Gong-Jun, Hu Xiao-Ya, Yan Chao
College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou, P. R. China.
Electrophoresis. 2009 Mar;30(6):1071-6. doi: 10.1002/elps.200800245.
Monolithic capillary columns were prepared by the reaction of a mixture of potassium silicate solution and formamide. The surface of the monolith was coated with a thin film formed by a sol-gel method to increase the surface area of the monolith and simultaneously covered with C8 as stationary phase for reversed-phase separation. The morphology of the monolithic column was investigated by SEM. Monolithic columns prepared in this manner showed high permeability and can be operated in capillary LC (CLC) mode at a pressure of 20 psi. PAHs were used to evaluate the separation performance of the stationary phase using CLC and pressurized CEC (pCEC). Efficiencies of 20 000 and 28 000 plates per meter for naphthalene were obtained in CLC and pCEC modes, respectively. Improvement in column efficiency and reduction in analysis time over CLC and improvement in operation facility and separation selectivity over CLC were found using pCEC mode.
通过硅酸钾溶液和甲酰胺的混合物反应制备整体式毛细管柱。整体柱的表面通过溶胶 - 凝胶法形成的薄膜进行涂覆,以增加整体柱的表面积,同时用C8作为反相分离的固定相进行覆盖。通过扫描电子显微镜(SEM)研究整体柱的形态。以这种方式制备的整体柱显示出高渗透性,并且可以在20 psi的压力下以毛细管液相色谱(CLC)模式运行。使用多环芳烃(PAHs)通过CLC和加压毛细管电色谱(pCEC)来评估固定相的分离性能。在CLC和pCEC模式下,萘的柱效分别为每米20000和28000理论塔板数。发现使用pCEC模式相对于CLC提高了柱效并缩短了分析时间,相对于CLC改善了操作便利性和分离选择性。