Micro-bore titanium housed polymer monoliths for reversed-phase liquid chromatography of small molecules |
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Authors: | Ekaterina P. Nesterenko Pavel N. Nesterenko Damian Connolly Flavie Lacroix Brett Paull |
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Affiliation: | 1. Irish Separation Science Cluster, National Centre for Sensor Research, Dublin City University, Glasnevin, Dublin 9, Ireland;2. Australian Centre for Research on Separation Science, University of Tasmania, Hobart, Tasmania 7001, Australia;3. Centre d’études superieures d’ingénieurs, 297, Rue de Vaugirard-75015, Paris, France |
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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 °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 μL/min and temperature of 110 °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. |
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Keywords: | Titanium column Polymer monolith High pressure reversed-phase HPLC |
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