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An alternative method for the sensitive determination of several drugs Of abuse and some of their metabolites in surface and sewage water samples is proposed Analytes are concentrated using a solid-phase extraction (SPE) sorbent, converted into the corresponding trimethylsilyl derivatives and selectively determined by gas chromatography (GC) with tandem mass spectrometry (MS/MS) detection Parameters affecting the performance of extraction, derivatisation and determination steps are systematically investigated Moreover, the stability of target analytes in sewage water samples is discussed Under final working conditions, water samples were adjusted at pH 8 5 and concentrated using a 200 mg OASIS HLB SPE cartridge Analytes were sequentially eluted with ethyl acetate followed by acetone and silylated using N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) The reaction was completed in 60 min at 80 degrees C and the mixture injected directly in the GC-MS/MS system without further purification in most cases, analytes presented a poor stability in sewage water samples, however. once they are submitted to the SPE process, cartridges can be stored at -20 degrees C for at least 3 Months Without significant degradation and/or inter-conversion reactions of illicit drugs The proposed method provided recoveries over 74% and LODs between 0 8 and 15 ng/L for rivet and treated wastewater samples In the case of raw wastewater slightly worse recoveries, between 63 and 137%. and similar LODs were attained Analysis of a limited number of waste and Surface water samples confirmed the presence of several illicit drugs ill the aquatic environment. with the highest levels and frequency corresponding to benzoylecgonine, the main metabolite of cocaine (C) 2010 Elsevier B V All rights reserved