title: Micro-bore titanium housed polymer monoliths for reversed-phase liquid chromatography of small molecules.
abstract: A new method for the fixation of polymethacrylate monoliths within titanium tubing of up to 0.8 mm I.D. for use as a chromatographic column under elevated temperatures and pressures is described. The preparation of butyl methacrylate-ethylene dimethacrylate-based monolithic stationary phases with desired porous structures was achieved within titanium tubing with pre-oxidised internal walls. The oxidised titanium surface was subsequently silanised with 3-trimethoxysilylpropyl methacrylate resulting in tight bonding of butyl methacrylate porous monolith to the internal walls, providing stationary phase stability at column temperatures up to 110 degrees C and at operating column pressure drops of >28 MPa. The titanium housed monoliths exhibited a uniform and dense porous structure, which provided peak efficiencies of up to 59,000 theoretical plates per meter when evaluated for the separation of small molecules in reversed-phase mode, under optimal conditions (achieved at 15 microL/min and temperature of 110 degrees C for naphthalene with a retention factor, k=0.58). The developed column was applied to the reversed-phase isocratic separation of a text mixture of pesticides.
authors.affiliation: Irish Separation Science Cluster, National Centre for Sensor Research, Dublin City University, Glasnevin, Dublin 9, Ireland.
authors.forename: Ekaterina P
authors.initials: EP
authors.lastname: Nesterenko
authors.forename: Pavel N
authors.initials: PN
authors.lastname: Nesterenko
authors.forename: Damian
authors.initials: D
authors.lastname: Connolly
authors.forename: Flavie
authors.initials: F
authors.lastname: Lacroix
authors.forename: Brett
authors.initials: B
authors.lastname: Paull
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D008689:Methacrylates / Q000737:chemistry*; D008855:Microscopy, Electron, Scanning; D009942:Organometallic Compounds / Q000737:chemistry; D010316:Particle Size; D010575:Pesticides / Q000302:isolation & purification; D016062:Porosity; D011312:Pressure; D015203:Reproducibility of Results; D013696:Temperature; D014025:Titanium / Q000737:chemistry*
chemical_list: D000097:Acetonitriles; D008689:Methacrylates; D009942:Organometallic Compounds; D010575:Pesticides; C004919:ethylene dimethacrylate; D014025:Titanium; C016284:butyl methacrylate; C032159:acetonitrile