Trace-level determination of pharmaceutical residues by LC-MS/MS in natural and treated waters. A pilot-survey study
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A pilot-survey study was performed by collecting samples (influent and effluent wastewaters, rivers and tap waters) from different locations in Europe (Spain, Belgium, Germany and Slovenia). A solid-phase extraction (SPE) followed by liquid chromatography–tandem mass spectrometry method was applied for the determination of pharmaceuticals (ibuprofen, naproxen, ketoprofen, diclofenac and clofibric acid). Method detection limits and method quantification limits were at the parts-per-trillion level (7.5–75 ng/L). The recovery rates of the SPE from deionized water and effluent wastewater samples spiked at 100- and 1,000-ng/L levels ranged from 87 to 95%. Identification criteria in compliance with the EU regulation for confirmatory methods of organic residues were applied. A detailed study of signal suppression evaluation for analysis of pharmaceutical residues in effluent wastewaters is presented.
KeywordsPharmaceuticals Natural water Treated water Liquid chromatography–tandem mass spectrometry
This study was financially supported by the European Commission Project (P-THREE no. EVK1-CT2002-0116, QUA-NAS—Improving the Infrastructure for Metrology in Chemistry in the Candidate New Member States, 5.OP EU, Competitive and Substainable Growth Programme, GTC1-2002-73003) and the Spanish Ministerio de Educación y Ciencia Project EVITA (CTM2004-06255-CO3-01 and PPQ2002-10945-E). The authors thank Merck for supplying LC columns. M.D.H. acknowledges the research contract (contrato de retorno de investigadores) from the Consejería de Educación y Ciencia de la Junta de Andalucía, Spain. M.P. acknowledges the ICREA contract from the Catalan Institution for Research and Advance Studies, and the Centro Superior de Investigaciones Científicas (CSIC), Barcelona, Spain. The authors also wish to thank R. Chaler and D. Fangul for their kind support with LC-MS/MS analysis.
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