title: A hybrid fluorous monolithic capillary column with integrated nanoelectrospray ionization emitter for determination of perfluoroalkyl acids by nano-liquid chromatography-nanoelectrospray ionization-mass spectrometry/mass spectrometry.
abstract: A hybrid fluorous monolithic column was simply prepared via photo-initiated free radical polymerization of an acrylopropyl polyhedral oligomeric silsesquioxane (acryl-POSS) and a perfluorous monomer (2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl acrylate) in UV-transparent fused-silica capillaries within 5min. The physical characterization of hybrid fluorous monolith, including scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, mercury intrusion porosimetry (MIP) and nitrogen adsorption/desorption measurement was performed. Chromatographic performance was also evaluated by capillary liquid chromatography (cLC). Due to the fluorous-fluorous interaction between fluorous monolith and analytes, fluorobenzenes could well be separated, and the column efficiencies reached 86,600-92,500plates/m at the velocity of 0.87mm/s for alkylbenzenes and 51,900-76,000plates/m at the velocity of 1.10mm/s for fluorobenzenes. Meanwhile, an approach to integrate nanoelectrospray ionization (ESI) emitter with hybrid fluorous monolithic column was developed for quantitative determination of perfluoroalkyl acids by nanoHPLC-ESI-MS/MS. The integration design could minimize extracolumn volume, thus excluding undesirable peak broadening and improving separation performance.
authors.affiliation: Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China; Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi'an 710069, China.
authors.forename: Haiyang
authors.initials: H
authors.lastname: Zhang
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 Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi'an 710069, China. Electronic address: ymwei@nwu.edu.cn.
authors.forename: Yinmao
authors.initials: Y
authors.lastname: Wei
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; 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. Electronic address: hanfazou@dicp.ac.cn.
authors.forename: Hanfa
authors.initials: H
authors.lastname: Zou
mesh_terms: D000143:Acids / Q000032:analysis; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation* / Q000379:methods*; D002853:Chromatography, Liquid; D004785:Environmental Pollutants / Q000032:analysis*; D005466:Fluorocarbons / Q000032:analysis*; D005609:Free Radicals; D008855:Microscopy, Electron, Scanning; D058105:Polymerization; D012822:Silicon Dioxide / Q000737:chemistry; D017550:Spectroscopy, Fourier Transform Infrared; D053719:Tandem Mass Spectrometry
chemical_list: D000143:Acids; D004785:Environmental Pollutants; D005466:Fluorocarbons; D005609:Free Radicals; D012822:Silicon Dioxide
keywords: Capillary liquid chromatography; Hybrid fluorous monolith; Integrated nanoelectrospray ionization emitter; Perfluoroalkyl acids