title: Facile construction of macroporous hybrid monoliths via thiol-methacrylate Michael addition click reaction for capillary liquid chromatography.
abstract: A facile approach based on thiol-methacrylate Michael addition click reaction was developed for construction of porous hybrid monolithic materials. Three hybrid monoliths were prepared via thiol-methacrylate click polymerization by using methacrylate-polyhedral oligomeric silsesquioxane (POSS) (cage mixture, n=8, 10, 12, POSS-MA) and three multi-thiol crosslinkers, 1,6-hexanedithiol (HDT), trimethylolpropane tris(3-mercaptopropionate) (TPTM) and pentaerythritol tetrakis(3-mercaptopropionate) (PTM), respectively, in the presence of porogenic solvents (n-propanol and PEG 200) and a catalyst (dimethylphenylphosphine, DMPP). The obtained monoliths possessed high thermal and chemical stabilities. Besides, they all exhibited high column efficiencies and excellent separation abilities in capillary liquid chromatography (cLC). The highest column efficiency could reach ca. 195,000N/m for butylbenzene on the monolith prepared with POSS-MA and TPTM (monolith POSS-TPTM) in reversed-phase (RP) mode at 0.64mm/s. Good chromatographic performance were all achieved in the separations of polycyclic aromatic hydrocarbons (PAHs), phenols, anilines, EPA 610 as well as bovine serum albumin (BSA) digest. The high column efficiencies in the range of 51,400-117,000N/m (achieved on the monolith POSS-PTM in RP mode) convincingly demonstrated the high separation abilities of these thiol-methacrylate based hybrid monoliths. All the results demonstrated the feasibility of the phosphines catalyzed thiol-methacrylate Michael addition click reaction in fabrication of monolithic columns with high efficiency for cLC applications.
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
authors.forename: Hui
authors.initials: H
authors.lastname: Lin
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; 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, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, 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.
authors.forename: Jing
authors.initials: J
authors.lastname: Dong
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: D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002853:Chromatography, Liquid; D057930:Click Chemistry; D058105:Polymerization; D013438:Sulfhydryl Compounds / Q000737:chemistry
chemical_list: D013438:Sulfhydryl Compounds
keywords: Capillary liquid chromatography; Click chemistry; Hybrid monolith; Polyhedral oligomeric silsesquioxane (POSS); Thiol-methacrylate Michael addition reaction