A hydrophobic organo-silica monolith containing octadecyl functionality was prepared via thermal polymerization from 3-(trimethoxysilyl)propyl methacrylate (MPTMS) with octadecyl methacrylate (ODM) in a presence of a crosslinker, ethylene dimethacrylate (EDMA). In contrast, thiol-ene click polymerization of MPTMS in presence of 1-octadecanethiol (ODT) and 2,2’-(ethylenedioxy)diethanolthiol (EDDT) resulted in a formation of soft gel. Further substitution of EDDT with 1,6-hexanedithiol (HDT) did not support formation of a monolith either. After adjusting the ratio of MPTMS to EDMA and MPTMS to ODM, useful monoliths were produced. Monolithic capillary columns were then tested for separation of selected analytes in reversed-phase liquid chromatography mode using aqueous acetonitrile as the mobile phase. These columns exhibited enhanced retention of alkylbenzenes compared to capillary columns prepared from MPTMS alone confirming the availability of octadecyl functionalities at the pore surface. Our “single-pot” approach eliminates the need for surface modification and therefore represents a faster alternative to preparation of hydrophobic organo-silica monolithic columns from 3-(trimethoxysilyl)propyl methacrylate.

Single-pot approach to preparation of hydrophobic sol-gel monolithic capillary columns for reversed-phase liquid chromatography

251st National Meeting (2016)

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