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Silica hybrid monolithic columns were prepared using two precursors, in which organo-functionalized trialkoxysilanes are mixed with tetraalkoxysilanes. In this study, several types of amino-functionalized silica hybrid monolithic columns were prepared via single-step “one-pot” approach, and the amount of silica precursors, porogens, as well as the reaction conditions were optimized. The preparation was carried out by mixing the silica precursors, i.e. tetraethoxysilane (TEOS) or tetramethoxysilane (TMOS) with amino precursors such as aminopropyltrimethoxysilane (APTES), aminoethylaminopropyl-trimethoxysilane (AEAPTMS), and phenylaminopropyltrimethoxysilane (PAPTMS) in a porogenic solution. The chromatographic performance of these hybrid monolithic columns was optimized by investigating several parameters through the separation of inorganic anions (IO3-, BrO3-, Br-, NO2-, NO3-, I-, SCN-) and some polar compounds (thymine, thymidine, adenosine, adenine, uridine). Results showed that the silica hybrid monolithic columns could be operated at higher flow-rate that favors rapid separation. The run-to-run repeatability of Si-APTES and Si-PAPTMS hybrid monolithic columns were satisfactory with relative standard deviations (n = 5) of less than 8% for all the analyte anions.

One-pot Facile Preparation of Amino-functionalized Silica Hybrid Monoliths for Mixed-mode Chromatography