School of Chemical and Biomedical Engineering, Nanyang Technological University, Singapore, Singapore.
Electrophoresis. 2010 Jan;31(2):378-87. doi: 10.1002/elps.200900318.
Rapid and efficient enantioseparation of halogen aryl alcohols and beta-blockers propranolol and pindolol in packed bed CEC (p-CEC) using as-prepared submicron porous silica chiral stationary phases (CSPs) has been achieved. Monodispersed 0.66 and 0.81 microm chiral submicron porous silica spheres were prepared using tetramethoxysilane and hexadecyltrimethylammonium bromide, followed by a hydrothermal treatment method with ammonia-ethanol to expand the pore of silica spheres without changing their spherical morphology. A proper specific surface of ca. 230 m(2)/g and pore sizes average of 6-8 nm were obtained by this method. The submicron porous silica spheres were modified with mono-6-phenylcarbamoylated beta-CD via thiol-en radical addition. They were packed into 9 cm 50 microm id capillary columns with photopolymerized monolithic frits. These submicron CSPs showed greater column efficiency (about 476 000 plates/m for 4-iodophenyl-1-ethanol) and higher resolution than the corresponding 3 microm CSP.
使用制备的亚微米多孔硅胶手性固定相（CSP），在填充床毛细管电色谱（p-CEC）中实现了卤代芳基醇、β受体阻滞剂普萘洛尔和吲哚洛尔的快速高效对映体分离。采用正硅酸四乙酯和十六烷基三甲基溴化铵制备了单分散的 0.66 和 0.81 微米手性亚微米多孔硅胶球，然后采用氨-乙醇水热处理法在不改变其球形形态的情况下扩大硅胶球的孔。通过该方法获得了约 230 m²/g 的适当比表面积和 6-8 nm 的平均孔径。通过巯基-烯自由基加成法将单-6-苯甲酰氨基-β-CD 修饰到亚微米多孔硅胶球上。它们被填充到带有光聚合整体式毛毡的 9 cm×50 µm id 毛细管柱中。这些亚微米 CSP 的柱效（4-碘苯-1-乙醇的柱效约为 476 000 板/m）和分辨率均高于相应的 3 µm CSP。
