title: Bridged polysilsesquioxane-based wide-bore monolithic capillary columns for hydrophilic interaction chromatography.
abstract: The synthesis and characterization of large-bore silica-based monolithic capillary columns (0.32mm×150mm) are presented. Columns were prepared by acidic hydrolysis of a mixture containing tetramethoxysilane (TMOS) and 1,2-bis(trimethoxysilyl)ethane (BTME) in different molar ratios in the presence of polyethylene glycol and urea. The monoliths were modified by zwitterionic monomer [2-(methacryloyloxy)ethyl]-dimethyl-(3-sulfopropyl)-ammonium hydroxide via 3-(trimethoxysilyl)propyl methacrylate. Prepared stationary phases were evaluated by scanning electron microscopy and chromatographic separation of nucleobases and their derivatives in the HILIC mode. The best chromatographic results were obtained with the column prepared from the reaction mixture containing BTME and TMOS in a 1:4 molar ratio. The permeability of such column reached 1.68×10-14m2and the efficiency, expressed as a height equivalent of the theoretical plate, did not exceed 10.5μm for the tested compounds. The columns were successfully applied to HILIC separation of native and labeled oligosaccharides and glycans released from bovine ribonuclease B and human immunoglobulin G.
authors.affiliation: Institute of Analytical Chemistry of the CAS, v. v. i., Veveří 97, 60200 Brno, Czechia.
authors.forename: Jozef
authors.initials: J
authors.lastname: Šesták
authors.affiliation: Institute of Analytical Chemistry of the CAS, v. v. i., Veveří 97, 60200 Brno, Czechia. Electronic address: moravcova@iach.cz.
authors.forename: Dana
authors.initials: D
authors.lastname: Moravcová
authors.affiliation: Institute of Analytical Chemistry of the CAS, v. v. i., Veveří 97, 60200 Brno, Czechia.
authors.forename: Jana
authors.initials: J
authors.lastname: Křenková
authors.affiliation: Institute of Analytical Chemistry of the CAS, v. v. i., Veveří 97, 60200 Brno, Czechia.
authors.forename: Josef
authors.initials: J
authors.lastname: Planeta
authors.affiliation: Institute of Analytical Chemistry of the CAS, v. v. i., Veveří 97, 60200 Brno, Czechia.
authors.forename: Michal
authors.initials: M
authors.lastname: Roth
authors.affiliation: Institute of Analytical Chemistry of the CAS, v. v. i., Veveří 97, 60200 Brno, Czechia.
authors.forename: František
authors.initials: F
authors.lastname: Foret
mesh_terms: D000818:Animals; D002417:Cattle; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D004980:Ethane / Q000031:analogs & derivatives / Q000737:chemistry; D006801:Humans; D057927:Hydrophobic and Hydrophilic Interactions; D007074:Immunoglobulin G / Q000378:metabolism; D008689:Methacrylates / Q000737:chemistry; D008855:Microscopy, Electron, Scanning; D009844:Oligosaccharides / Q000032:analysis / Q000302:isolation & purification; D017646:Organosilicon Compounds / Q000737:chemistry*; D012260:Ribonucleases / Q000378:metabolism; D012822:Silicon Dioxide / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization; D014297:Trimethylsilyl Compounds / Q000737:chemistry
chemical_list: D007074:Immunoglobulin G; D008689:Methacrylates; D009844:Oligosaccharides; D017646:Organosilicon Compounds; D014297:Trimethylsilyl Compounds; C517344:bis(trimethoxysilyl)ethane; C569780:polysilsesquioxane; D012822:Silicon Dioxide; D012260:Ribonucleases; C029600:ribonuclease B; C505504:3-(trimethoxysilyl)propyl methacrylate; D004980:Ethane
keywords: HILIC; Nucleosides; Oligosaccharides; Silica monolithic column