Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1217, Issue 14, Pages 2138-2146Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2010.02.007
Keywords
Titanium column; Polymer monolith; High pressure reversed-phase HPLC
Funding
- Science Foundation Ireland [08/SRC/B1412]
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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 mu L/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. (C) 2010 Elsevier B.V. All rights reserved.
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