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The occurrence of polar pesticides in sediments has not been extensivelyinvestigated because of their relatively poor hydrophobicity and apparentlyless persistence in the environment. However, their continuous release into theaquatic systems calls for the evaluation of their potential accumulation insediments and the role of this matrix as a potential source of these compounds.Considering this, a method based on pressurized liquid extraction (PLE),extract clean-up by solid phase extraction (SPE) and analyte determination byliquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) wasdeveloped and validated to analyze 50 relevant (frequently used and/orregulated or found in water) medium to highly polar pesticides in sediments.The method showed good performance regarding accuracy (relative recoveriesbetween 76% and 124%), precision (relative standard deviation values <20%),sensitivity (LODs in the low ng/g for most compounds), linearity (coefficientsof determination >0.99), and matrix effects (negligible for all analytes). Theuse of an isotope dilution approach for quantification ensures resultsreliability. As a part of the validation process, the method was applied to theanalysis of the target pesticides in sediments from the Llobregat River (NESpain) showing the presence of five of them, namely, terbutryn, dichlorvos,terbuthylazine, diazinon, and irgarol. All 5 pesticides, due to both theconcentrations found and their physical-chemical characteristics, demonstratehigh potential for bioaccumulation and risk to the aquatic organisms.Additional multidisciplinary studies that investigate pesticides occurrence inthe different aquatic compartments and evaluate the potential risks for aquaticecosystems are required to assess the environmental impact and significance ofthe presence of pesticides in sediments.

analytical and bioanalytical chemistry/analytical and bioanalytical chemistry

Reliable LC-MS/MS-based method for trace level determination of 50  medium to highly polar pesticide residues in sediments and ecological risk  assessment