Author(s): VazquezRoig P, Segarra R, Blasco C, Andreu V, Pic Y
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Abstract The present work describes the development of a sensitive analytical method based on pressurized liquid extraction (PLE) and pre-concentration by solid-phase extraction (SPE), followed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seventeen pharmaceuticals in soils and sediments. The method is based on sample homogenisation using Na(2)-EDTA washed sand and extraction with water at 90 degrees C. Special emphasis was placed on the optimization of the extraction procedure to develop a green method that reduces, at a maximum, the use of organic solvents in order to eliminate matrix components during the clean-up. The proposed method was linear in a concentration range from 0.3 to 333ngg(-1), with correlation coefficients higher than 0.993. Method detection (MDLs) and quantification (MQLs) limits ranged from 0.1 to 6.8ngg(-1) and from 0.25 to 23ngg(-1), respectively. Absolute recoveries were analyte dependent, varying between 50\% and 105\% at the MQL level, except for fenofibrate (40\%) and diclofenac (34\%). The intra-day and inter-day precision was given by RSD values from 0.7\% to 7.9\% and from 1.6\% to 14.5\%, respectively. Acetaminophen, carbamazepine, ciprofloxacin, clofibric acid, codeine, diazepam, fenofibrate, metropolol, ofloxacin and propanolol were detected at concentrations from MDL to 35.62ngg(-1) in soils and sediments from marsh areas. Due to the low recoveries, results for fenofibrate and diclofenac can only be considered as semi-quantitative. The method was fully suitable for the other 15 pharmaceuticals. Copyright 2009 Elsevier B.V. All rights reserved.
This article was published in J Chromatogr A
and referenced in Pharmaceutica Analytica Acta