title: Chromatographic efficiency comparison of polyhedral oligomeric silsesquioxanes-containing hybrid monoliths via photo- and thermally-initiated free-radical polymerization in capillary liquid chromatography for small molecules.
abstract: Monolithic poly(methacrylate epoxy cyclosiloxane-co-polyhedral oligomeric silsesquioxanes) (epoxy-MA-POSS) capillary columns have been prepared via either photo- or thermally-initiated polymerization of the corresponding monomers using a 1-propanol/PEG 400 mixture as porogens. Photochemical polymerization was accomplished by irradiation of the UV-transparent capillary for 10min at room temperature, while thermal polymerization was performed at 55°C, 60°C or 65°C for 18h. The evaluation of chromatographic property for two hybrid epoxy-MA-POSS monoliths was carried out. The results indicate that hybrid monoliths fabricated by photochemical initiation exhibit higher column efficiency (97,000-98,400plates/m) than those synthesized by thermal polymerization (41,100-48,000plates/m) in cLC. The higher efficiency of photo-initiated hybrid monoliths is closely related to lower eddy dispersion (A-term) and mass transfer resistance (C-term).
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China; State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024, China.
authors.forename: Hongwei
authors.initials: H
authors.lastname: Wang
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. Electronic address: junjieou@dicp.ac.cn.
authors.forename: Junjie
authors.initials: J
authors.lastname: Ou
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
authors.forename: Zhongshan
authors.initials: Z
authors.lastname: Liu
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
authors.forename: Hui
authors.initials: H
authors.lastname: Lin
authors.affiliation: State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024, China.
authors.forename: Xiaojun
authors.initials: X
authors.lastname: Peng
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. Electronic address: hanfazou@dicp.ac.cn.
authors.forename: Hanfa
authors.initials: H
authors.lastname: Zou
mesh_terms: D000098:Acetophenones; D001555:Benzene Derivatives / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods*; D004852:Epoxy Compounds / Q000737:chemistry*; D005609:Free Radicals; D006358:Hot Temperature; D017646:Organosilicon Compounds / Q000737:chemistry*; D055668:Photochemical Processes; D058105:Polymerization; D011109:Polymethacrylic Acids / Q000737:chemistry*
chemical_list: D000098:Acetophenones; D001555:Benzene Derivatives; D004852:Epoxy Compounds; D005609:Free Radicals; D017646:Organosilicon Compounds; D011109:Polymethacrylic Acids; C452198:2,2-dimethoxy-2-phenylacetophenone
keywords: 2,2-Dimethoxy-2-phenylacetophenone; Free-radical polymerization; Hybrid monoliths; Methacrylate epoxy cyclosiloxane; POSS; Photochemical initiation