title: Rapid "one-pot" preparation of polymeric monolith via photo-initiated thiol-acrylate polymerization for capillary liquid chromatography.
abstract: A facile approach was exploited for fast preparation of polymer-based monoliths in UV-transparent fused-silica capillaries via "one-pot" photo-initiated thiol-acrylate polymerization reaction of dipentaerythritolpenta-/hexaacrylate (DPEPA) and 1-octadecanethiol (ODT) in the presence of porogenic solvents (1-butanol and ethylene glycol). Due to relative insensitivity of oxygen inhibition in thiol-ene free-radical polymerization, the polymerization could be performed within 5 min. The effects of composition of prepolymerization solution on the morphology and permeability of poly(ODT-co-DPEPA) monoliths were investigated in detail by adjusting the content of monomer and binary porogen ratio. The physical properties of poly(ODT-co-DPEPA) monoliths were characterized by Fourier transform infrared spectroscopy (FT-IR), mercury intrusion porosimetry (MIP) and nitrogen adsorption/desorption measurement. The evaluation of chromatographic performance was carried out by capillary liquid chromatography (cLC). The results indicated that the poly(ODT-co-DPEPA) monolith was homogeneous and permeable, and also possessed a typical reversed-phase retention mechanism in cLC with high efficiency (∼75,000 N m(-1)) for separation of alkylbenzenes. Eventually, the further separation of tryptic digest of proteins by cLC tandem mass spectrometry (cLC-MS/MS) demonstrated its potential in the analysis of biological samples.
authors.affiliation: Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Shaanxi Alcohol Ether and Biomass Energy Engineering Research Center, Key Laboratory of Yulin Desert Plants Resources, Xi'an 710069, China; Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China.
authors.forename: Jingyao
authors.initials: J
authors.lastname: Bai
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China.
authors.forename: Hongwei
authors.initials: H
authors.lastname: Wang
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), 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, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China.
authors.forename: Zhongshan
authors.initials: Z
authors.lastname: Liu
authors.affiliation: Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Shaanxi Alcohol Ether and Biomass Energy Engineering Research Center, Key Laboratory of Yulin Desert Plants Resources, Xi'an 710069, China. Electronic address: yhshen@nwu.edu.cn.
authors.forename: Yehua
authors.initials: Y
authors.lastname: Shen
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China. Electronic address: hanfazou@dicp.ac.cn.
authors.forename: Hanfa
authors.initials: H
authors.lastname: Zou
mesh_terms: D000179:Acrylates / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods*; D058105:Polymerization; D011108:Polymers / Q000737:chemistry*; D013438:Sulfhydryl Compounds / Q000737:chemistry*
chemical_list: D000179:Acrylates; D011108:Polymers; D013438:Sulfhydryl Compounds
keywords: Capillary liquid chromatography; Photo-initiated thiol-acrylate polymerization; Polymeric monolith