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Alkanethiol‐functionalized organosilicon monoliths for nano‐reversed‐phase liquid chromatography
Author(s) -
Demir Cihan,
Kip Çiğdem,
Tuncel Ali
Publication year - 2018
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.201800280
Subject(s) - organosilicon , nano , chromatography , phase (matter) , chemistry , liquid phase , high performance liquid chromatography , reversed phase chromatography , materials science , organic chemistry , composite material , physics , thermodynamics
Organosilicon monoliths carrying chromatographic ligands with different alkyl chain lengths were obtained by thiol‐methacrylate photopolymerization. The use of thiol‐ene chemistry in the presence of a main monomer with a series of methacrylate functionality (i.e., methacrylate substituted polyhedral oligomeric silsesquioxane) allowed the synthesis of organosilicon monoliths with high cross‐linking density and carrying hydrophobic alkyl‐chain ligands by a one‐pot process. In the synthesis runs, 1‐butanethiol, 1‐octanethiol, and 1‐octadecanethiol were used as the hydrophobic thiol ligands with the number of methylene units between 4 and 18. The selectivity analysis performed using cytosine/uracil retention ratio showed that alkanethiol‐attached organosilicon monoliths exhibited hydrophobicity close to octadecyl‐attached silica‐based RP columns. In the RP, chromatographic runs performed in nano‐liquid chromatography, phenols, alkylbenzenes, and PAHs were used as the analytes. Among the synthesized monoliths, retention‐independent plate height behavior and the smallest plate heights were obtained with 1‐octadecanethiol‐attached organosilicon monolith for the analytes in a wide polarity range. With this monolith, the mobile phases prepared with ACN contents ranging between 35 and 85% v/v could be used for satisfactory separation of analytes in a wide polarity range.