title: Synthesis of a reactive polymethacrylate capillary monolith and its use as a starting material for the preparation of a stationary phase for hydrophilic interaction chromatography.
abstract: Poly(3-chloro-2-hydroxypropyl methacrylate-co-ethylene dimethacrylate), poly(HPMA-Cl-co-EDMA) capillary monolith was proposed as a reactive starting material with tailoring flexibility for the preparation of monolithic stationary phases. The reactive capillary monolith was synthesized by free radical copolymerization of 3-chloro-2-hydroxypropyl methacrylate (HPMA-Cl) and ethylene dimethacrylate (EDMA). The mean pore size, the specific surface area and the permeability of poly(HPMA-Cl-co-EDMA) monoliths were controlled by adjusting porogen/monomer volume ratio, porogen composition and polymerization temperature. The porogen/monomer volume ratio was found as the most effective factor controlling the porous properties of poly(HPMA-Cl-co-EDMA) monolith. Triethanolamine (TEA-OH) functionalized polymethacrylate monoliths were prepared by using the reactive chloropropyl group of poly(HPMA-Cl-co-EDMA) monolith via one-pot and simple post-functionalization process. Poly(HPMA-Cl-co-EDMA) monolith reacted with TEA-OH was evaluated as a stationary phase in nano-hydrophilic interaction chromatography (nano-HILIC). Nucleotides, nucleosides and benzoic acid derivatives were satisfactorily separated with the plate heights up to 20μm. TEA-OH attached-poly(HPMA-Cl-co-EDMA) monolith showed a reproducible and stable retention behaviour in nano-HILIC runs. However, a decrease in the column performance (i.e. an increase in the plate height) was observed with the increasing retention factor. Hence "retention-dependent column efficiency" behaviour was shown for HILIC mode using the chromatographic data collected with the polymer based monolith synthesized.
authors.affiliation: Hacettepe University, Chemical Engineering Department, Beytepe/Ankara, Turkey.
authors.forename: Çiğdem
authors.initials: Ç
authors.lastname: Kip
authors.affiliation: Hacettepe University, Chemical Engineering Department, Beytepe/Ankara, Turkey.
authors.forename: Damla
authors.initials: D
authors.lastname: Erkakan
authors.affiliation: Hacettepe University, Chemical Engineering Department, Beytepe/Ankara, Turkey.
authors.forename: Aslıhan
authors.initials: A
authors.lastname: Gökaltun
authors.affiliation: Hacettepe University, Chemical Engineering Department, Beytepe/Ankara, Turkey.
authors.forename: Bekir
authors.initials: B
authors.lastname: Çelebi
authors.affiliation: Hacettepe University, Chemical Engineering Department, Beytepe/Ankara, Turkey; Hacettepe University, Division of Nanotechnology & Nanomedicine, Ankara, Turkey. Electronic address: atuncel@hacettepe.edu.tr.
authors.forename: Ali
authors.initials: A
authors.lastname: Tuncel
mesh_terms: D001565:Benzoates / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000295:instrumentation*; D004983:Ethanolamines / Q000737:chemistry; D057927:Hydrophobic and Hydrophilic Interactions; D009705:Nucleosides / Q000302:isolation & purification; D009711:Nucleotides / Q000302:isolation & purification; D010539:Permeability; D058105:Polymerization; D011109:Polymethacrylic Acids / Q000138:chemical synthesis / Q000737:chemistry*; D016062:Porosity
chemical_list: D001565:Benzoates; D004983:Ethanolamines; D009705:Nucleosides; D009711:Nucleotides; D011109:Polymethacrylic Acids; C000600591:poly(HPMA-Cl-co-EDMA); C009546:triethanolamine
keywords: Chloromethyl group; Chromatographic separation; Liquid chromatography; Post-functionalization; Reactive monolith