One-step synthesis of sub-2 μm vinyl functionalized silica sphere as stationary phase for liquid chromatography

Yuming Xie; Xiaoqiong Zhang; Qiang Han; Wei Wan; Mingyu Ding

doi:10.1016/j.talanta.2014.11.044

One-step synthesis of sub-2 μm vinyl functionalized silica sphere as stationary phase for liquid chromatography

Talanta. 2015 Mar:134:425-434. doi: 10.1016/j.talanta.2014.11.044. Epub 2014 Nov 29.

Authors

Yuming Xie¹, Xiaoqiong Zhang¹, Qiang Han¹, Wei Wan¹, Mingyu Ding²

Affiliations

¹ Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China.
² Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China. Electronic address: dingmy@mail.tsinghua.edu.cn.

PMID: 25618689
DOI: 10.1016/j.talanta.2014.11.044

Abstract

Vinyl-functionalized silica spheres (VFSS) were synthesized through the one-step method. The effects of reactant ratio, temperature, reaction time and ammonium hydroxide dripping speed were investigated. The diameter of the spheres reached sub-2 μm magnitude by controlling the reaction conditions, which is suitable for high performance liquid chromatography (HPLC) packing material. The vinyl groups in the silica spheres were further successfully modified by octadecyl (C18) groups through a "thiol-ene" click reaction. Raw VFSS and C18modified VFSS (C-VFSS) were used as HPLC stationary phases to separate benzene homologs (benzene, toluene, and meta-xylene) and nonpolar compounds with different ring contents (benzene, phenantherene and fluoranthene). Both VFSS and C-VFSS exhibited hydrophobic retention behavior. Additionally, vinyl groups in the silica spheres may offer a π-π electron-donor-acceptor (EDA) retention mechanism for chromatographic separation.

Keywords: Cycle-model; High performance liquid chromatography; Stationary phase; Sub-2μm vinyl-functionalized silica sphere; Thiol-ene reaction.