Abstract
A multiresidue method for the fast and efficient analysis of current-use pesticides in streambed sediments is reported. The method employs pressurized liquid extraction (PLE) for the automated extraction of pesticide residues from small quantities (5 g) of lyophilized sediment samples. Various PLE parameters, including the extraction solutions and oven temperature, were optimized for thirty diverse current-use pesticides (CUPs) known to be commonly applied to corn and soybean monoculture crops. Following extraction, samples were analyzed with a fast and simplified quantitative multiresidue analytical method using ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) with online solid phase extraction (SPE) on a hydrophilic-lipophilic balance (HLB) column. Validation of the method demonstrated acceptable recoveries (avg 41.4 %) comparable with other multiresidue methods for sediments, reliable intraday (<13 %) and interday (<24 %) repeatability, reasonable matrix effects (avg −54 %), and low LODs (avg 0.53 ng g−1 dw) and LOQs (avg 2.18 ng g−1 dw) given the complexity of the sediment matrix. The method was applied to 119 streambed sediment samples collected from agriculture-adjacent headwater streams near Lac Saint-Pierre in Québec, Canada to demonstrate the utility of the method. Fourteen of the thirty target analytes were detected within the samples, including nine herbicides, two insecticides, and three fungicides. To the best of our knowledge, an equally simple and efficient multiresidue method for the quantitative analysis of diverse CUPs in streambed sediments using PLE and UHPLC-MS/MS with online SPE has not yet been reported in the literature. This method helps to reduce labour and material inputs, avoids excessive sample manipulation, and allows for fast quantitative analysis of trace pesticide residues in streambed sediments, with the potential for application to other contaminants of emerging concern.
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