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Dual gradient LC method for the determination of pharmaceutical residues in environmental samples using a monolithic silica reversed phase column

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Bones, J and Nesterenko, PN and Thomas, K and Paull, B (2006) Dual gradient LC method for the determination of pharmaceutical residues in environmental samples using a monolithic silica reversed phase column. International Journal of Environnmental Chemistry, 86 (7). pp. 487-504. ISSN 0306-7319

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Abstract

Detailed below is a simple reversed-phase liquid chromatography (RP-LC) method for the simultaneous separation of up to 21 acidic, basic, and neutral pharmaceuticals using Merck Chromolith Performance RP-C18e monolithic columns with direct ultraviolet (UV) absorption detection. By simultaneously applying a solvent elution gradient program with a mobile phase flow gradient, both a decrease in the overall analysis time and a general increase in peak efficiencies were observed. Mobile phase pH and buffer concentration were optimised using the overall resolution product under applied gradient conditions. Under optimised conditions peak area reproducibility (n = 6) ranged between 0.4 and 9.3%, determined at the method LOQ level. For real sample analysis pharmaceutical residues were extracted using an optimised solid phase extraction (SPE) procedure, utilising Strata-X extraction cartridges, which overall provided the highest relative recovery data in comparison with four other commercially available SPE sorbents (17 out of 20 residues investigated had recoveries over 70%). Complete method precision, including all sample pre-treatment and LC analysis for six spiked river water samples at the 1 and 2 µg L-1 level was between 10 and 29%. Using 1 L volumes of 1 µg L-1 spiked estuarine water samples, the majority of detection limits were found to be in the 10-50 ng L-1 range.

Item Type: Article
Keywords: monolithic silica; dual gradient; RP-LC; SPE; pharmaceuticals
Journal or Publication Title: International Journal of Environnmental Chemistry
Page Range: pp. 487-504
ISSN: 0306-7319
Identification Number - DOI: 10.1080/03067310500229635
Additional Information: The definitive published version is available online at: http://www.tandf.co.uk/journals
Date Deposited: 19 Sep 2008 04:16
Last Modified: 18 Nov 2014 03:50
URI: http://eprints.utas.edu.au/id/eprint/7559
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