title: One-step synthesis of sub-2 μm vinyl functionalized silica sphere as stationary phase for liquid chromatography.
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.
authors.affiliation: Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China.
authors.forename: Yuming
authors.initials: Y
authors.lastname: Xie
authors.affiliation: Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China.
authors.forename: Xiaoqiong
authors.initials: X
authors.lastname: Zhang
authors.affiliation: Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China.
authors.forename: Qiang
authors.initials: Q
authors.lastname: Han
authors.affiliation: Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China.
authors.forename: Wei
authors.initials: W
authors.lastname: Wan
authors.affiliation: Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China. Electronic address: dingmy@mail.tsinghua.edu.cn.
authors.forename: Mingyu
authors.initials: M
authors.lastname: Ding
keywords: Cycle-model; High performance liquid chromatography; Stationary phase; Sub-2μm vinyl-functionalized silica sphere; Thiol-ene reaction