Key Laboratory of Chemo/Biosensing & Chemometrics, College of Chemistry & Chemical Engineering, Hunan University, Changsha 410082, China.
Talanta. 2012 Mar 15;91:52-9. doi: 10.1016/j.talanta.2012.01.009. Epub 2012 Jan 12.
An n-octadecanethiol (C(18))/3-mercapto-1-propane-sulfonate (MPS) modified organic-inorganic hybrid silica monolithic column possessing vinyl ligands through thiol-ene click chemistry for capillary electrochromatography (CEC) is described. The proposed column is prepared via the sol-gel process by in situ co-condensation using vinyltrimethoxysilane (VTMS) and tetra-methoxysilane (TMOS) as precursors. Examination by SEM shows that the capillary has homogenous macroporous morphology and is well attached to the inner wall of the capillary. The obtained C(18)-MPS-VTMS silica hybrid monolithic column demonstrated an enhanced hydrophilic property and could be applied as a reversed-phase stationary phase in CEC directly. Compared with unmodified VTMS silica hybrid monolithic column, stronger EOF was observed using this monolithic column. VTMS/TOMS ratios in the reaction mixture were varied and 1:3 was found to be optimum. Good separations of benzenes, aromatic amines, acids and peptides were achieved, the lowest plate height of ≈ 3μm was obtained, the peak symmetry range from 0.98 to 1.29. The resulting C(18)-MPS-VTMS silica hybrid monolithic column can be used in different separation modes, including reversed phase mode and ion exchange mode.
一种十八烷硫醇（C（18））/3-巯基-1-丙磺酸（MPS）修饰的有机-无机杂化硅胶整体柱，通过硫醇-烯点击化学具有乙烯基配体，用于毛细管电色谱（CEC）。该柱是通过溶胶-凝胶过程原位共缩合，以乙烯基三甲氧基硅烷（VTMS）和四甲氧基硅烷（TMOS）为前体制备的。SEM 观察表明，毛细管具有均匀的大孔形貌，并且与毛细管的内壁很好地附着。所得的 C（18）-MPS-VTMS 硅胶杂化整体柱表现出增强的亲水性，可直接作为 CEC 中的反相固定相应用。与未改性的 VTMS 硅胶杂化整体柱相比，使用该整体柱观察到更强的EOF。在反应混合物中改变 VTMS/TOMS 比，发现 1:3 为最佳。实现了苯、芳香胺、酸和肽的良好分离，获得了最低的板高≈3μm，峰形从 0.98 到 1.29 不等。所得的 C（18）-MPS-VTMS 硅胶杂化整体柱可用于不同的分离模式，包括反相模式和离子交换模式。
