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Multiresidue determination and uncertainty analysis of pesticides in soil by ultrafast liquid chromatography coupled to mass spectrometry

This work presents the validation results of a simple, fast and low-cost sample preparation method for the determination of pesticide residues in soil by ultrafast liquid chromatography coupled to electrospray ionization mass spectrometry. The method uses acetonitrile ultrasound-assisted extraction, centrifugation and evaporation step, without further cleanup. Recovery studies were performed for two soil blanks, presenting results in the range of 70-110% with relative standard deviation lower than 20%. The correlation coefficients for analytical calibration curves were higher than 0.99. Pesticide residues were detected in soils in the range of 1-62 ng g-1, depending on the compound. The uncertainty of the method was estimated from different addition-recovery experiments and calculations from certificates. The extraction process was identified as the main source of uncertainty, and the expanded uncertainties for each pesticide, using a coverage factor of two, were between 8.4 and 33%. The proposed method was applied to the determination of pesticides in real samples.

pesticide; mass spectrometry; liquid chromatography; soil


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