title: Capillary methacrylate-based monoliths by grafting from/to γ-ray polymerization on a tentacle-type reactive surface for the liquid chromatographic separations of small molecules and intact proteins.
abstract: Capillary methacrylate-based monoliths were prepared for the high performance liquid chromatography (HPLC) separation of both small molecules and large biomolecules. An efficient grafting from/to synthetic approach was adopted introducing a network of activated sites in the inner wall surface using the new silanization agent (N-trimethoxysilylpropyl)-polyethylenimine. Copolymerization of lauryl methacrylate monomer and 1,6-hexanediol dimethacrylate cross-linker in the presence of porogenic solvents was obtained under continuous γ-ray exposure with high conversion yield. The morphology and porous structure of the resulting monoliths have been investigated by Scanning Electron Microscopy (SEM) and1H NMR cryoporosimetry. By chromatographic investigation, the new capillary columns attested high kinetic performance (with efficiency larger than 100,000 theoretical plate/m for small molecules at optimum mobile phase linear velocity of about 0.5mm/s) and also excellent mechanical stability and repeatability. The new methacrylate-based monolithic capillary columns have been successfully employed for efficient reversed-phase separation of intact proteins and peptides.
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P. le Aldo Moro 5, 00185 Roma Italy.
authors.forename: Patrizia
authors.initials: P
authors.lastname: Simone
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P. le Aldo Moro 5, 00185 Roma Italy.
authors.forename: Giuseppe
authors.initials: G
authors.lastname: Pierri
authors.affiliation: Istituto di Metodologie Chimiche, Area della Ricerca di Roma del CNR, Monterotondo Stazione, 00016 Roma Italy.
authors.forename: Donatella
authors.initials: D
authors.lastname: Capitani
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P. le Aldo Moro 5, 00185 Roma Italy.
authors.forename: Alessia
authors.initials: A
authors.lastname: Ciogli
authors.affiliation: Istituto di Metodologie Chimiche, Area della Ricerca di Roma del CNR, Monterotondo Stazione, 00016 Roma Italy.
authors.forename: Giancarlo
authors.initials: G
authors.lastname: Angelini
authors.affiliation: Istituto di Metodologie Chimiche, Area della Ricerca di Roma del CNR, Monterotondo Stazione, 00016 Roma Italy.
authors.forename: Ornella
authors.initials: O
authors.lastname: Ursini
authors.affiliation: Istituto per i Polimeri Compositi e Biomateriali, Consiglio Nazionale delle Ricerche, Via Campi Flegrei 34, 80078 Pozzuoli Italy.
authors.forename: Gennaro
authors.initials: G
authors.lastname: Gentile
authors.affiliation: Dipartimento di Scienze Chimiche e Farmaceutiche, Università di Ferrara, via L. Borsari 46, 44121 Ferrara, Italy.
authors.forename: Alberto
authors.initials: A
authors.lastname: Cavazzini
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P. le Aldo Moro 5, 00185 Roma Italy.
authors.forename: Claudio
authors.initials: C
authors.lastname: Villani
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P. le Aldo Moro 5, 00185 Roma Italy. Electronic address: francesco.gasparrini@uniroma1.it.
authors.forename: Francesco
authors.initials: F
authors.lastname: Gasparrini
mesh_terms: D002623:Chemistry Techniques, Analytical / Q000295:instrumentation / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D005720:Gamma Rays; D008689:Methacrylates / Q000737:chemistry*; D010455:Peptides / Q000302:isolation & purification*; D058105:Polymerization; D016062:Porosity; D011506:Proteins / Q000302:isolation & purification*; D012997:Solvents / Q000737:chemistry
chemical_list: D008689:Methacrylates; D010455:Peptides; D011506:Proteins; D012997:Solvents; C115846:dodecyl methacrylate; C090921:1,6-hexanediol dimethacrylate
keywords: Biomolecule separation; Capillary high performance liquid chromatography; Monolith morphology; Organic polymer monoliths