Fast fabrication of a hybrid monolithic column containing cyclic and aliphatic hydrophobic ligands via photo-initiated thiol-ene polymerization

J Sep Sci. 2019 Apr;42(7):1332-1340. doi: 10.1002/jssc.201801033. Epub 2019 Feb 5.

Abstract

Three monomers, octakis (3-mercaptopropyl) octasilsesquioxane, 1,2,4-trivinylcyclohexane and isophytol were employed to synthesize a novel monolithic stationary phase via photo-initiated thiol-ene click polymerization for reversed-phase liquid chromatography. Several factors such as porogenic system, reaction time and the molar ratio of functional groups were investigated in detail. The resulting poly(POSS-co-TVCH-co-isophytol) monolithic column exhibited suitable permeability for fast separation and outstanding thermal stability. Five alkylbenzenes were employed to evaluate the ability of chromatographic separation of the resulting monolithic columns at different flow rates, and showed the highest column efficiencies of 90,200-93,100 N/m (corresponding to 10.4-10.6 μm of plate height) at a velocity of 0.41 mm/s. The baseline separations of five anilines and eight phenols further proved the applicability of poly(POSS-co-TVCH-co-isophytol) monolithic column in the separation of small molecules.

Keywords: capillary liquid chromatography; click chemistry; hybrid monolithic column.