Journal
TALANTA
Volume 70, Issue 5, Pages 1117-1128Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2006.02.026
Keywords
pharmaceuticals; LC-UV-ESI-MS; on-line SPE; preconcentration; monolithic reversed-phase silica
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A simplified preconcentration method for a range of ultra-trace level pharmaceuticals in natural waters has been developed. Solid phase extraction was performed on-line using a micro-reversed-phase monolithic silica column, allowing for very rapid trace enrichment front large Volume (500 ml) samples with minimal sample handling. Acceptable recoveries of > 70% were obtained for the majority of compounds investigated and the monolithic columns could be washed and conditioned on-line with no sample carryover and used reproducibly for up to eight extractions each. The on-line SPE-LC-UV method was coupled to electrospray ionisation ion trap mass spectrometry (ESI-MS) to increase both selectivity and specificity. Detection limits were determined in spiked river and tap water samples and found to lie in the low ng/l region using sample volumes of 500 ml., loaded at a flow rate of 10 ml/min, and therefore, were suitable for ultra trace analysis. (c) 2006 Elsevier B.V. All rights reserved.
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