Suchergebnisse

This work describes the optimization, validation and application to real samples of an ultra-high-pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for the quantification and confirmation of 11 compounds (atrazine, simazine, terbuthylazine, terbumeton, terbutryn and their main transformation products) in surface and wastewater samples. Most of these analytes are included in the list of priority substances in the framework on European Water Policy. The application of this method to water samples reveals that the most relevant transformation products (TPs) should be incorporated into current analytical methods (which are focused mainly on the determination of unchanged compounds), to obtain a more realistic knowledge on water quality regarding pesticide contamination. TPs are generally more polar and mobile than the parents and they can be transported to the aquatic environment more rapidly than their precursors. Additionally, they can present some degree of toxicity and in fact TPs are also included within the legislation on drinking water as pesticide derivatives. To efficiently combine UHPLC with MS/MS, a fast-acquisition triple quadrupole mass analyzer was used. Working in selected reaction monitoring mode, up to three simultaneous transitions per compound were acquired allowing a reliable identification at ng/L levels. The method developed includes a pre-concentration step based on solid-phase extraction (OASIS HLB cartridges). Satisfactory recoveries (70-120%) and relative standard deviations (<20%) were obtained for all compounds in different water samples types spiked at two concentration levels (0.025 and 0.1 μg/L). The optimized method was found to have excellent sensitivity with instrumental detection limits as low as 50 fg. In addition, the influences of the matrix constituents on ionization efficiency and extraction recovery have been studied in different types of Italian and Spanish surface and urban wastewater. Signal suppressions were observed for all compounds, ...