One pot synthesis of carboxyl functionalized-polyhedral oligomeric siloxane based monolith via photoinitiated thiol-methacrylate polymerization for nano-hydrophilic interaction chromatography.

A hybrid monolith exhibiting almost retention independent separation performance in hydrophilic interaction chromatography (HILIC) was obtained by one-pot photoinitiated thiol-methacrylate polymerization. Polyhedral oligomeric silsesquioxane containing methacrylate units (POSS-MA) was used as the main monomer and crosslinking agent, together with a hydrophilic ligand with two carboxyl groups, mercaptosuccinic acid (MSA) as the thiol agent and chromatographic ligand. The isocratic separation of nucleosides, nucleotides and organic acids on MSA attached-poly(POSS-MA) monolith was investigated in HILIC mode. The van-Deemter plots for obtained for nucleosides, nucleotides and benzoic acids clearly showed that there were two regions in each graph with two different slopes in the studied range of linear flow rate (i.e. 0.2-4.3mm/s). The slope of plate height-linear velocity curve was so small in the low linear velocity region between 0.2-2.1mm/s while the slope in high linear velocity region between 2.1-4.3mm/s was so higher with respect to the first region. The van-Deemter plots sketched for all analyte grous used in HILIC mode obeyed this tendency Almost "retention independent plate height behavior" was demonstrated in HILIC, using nucleotides, nucleotides or benzoic acids as the analytes in the linear velocity range of 0.2-2.1mm/s. This behavior was explained by the porous structure of the synthesized monolith facilitating the convective transport of analytes. The variation of plate height was not retention-independent within high linear velocity range (>3.2mm/s) when nucleosides were separated in HILIC mode.