A new sample preparation approach for the analysis of 98 current-use pesticides in soil and herbaceous vegetation using HPLC-MS/MS in combination with an acetonitrile-based extraction

Abstract

A simple acetonitrile-based extraction method for the determination of 98 current-use pesticides (CUPs) in soil and herbaceous vegetation using HPLC-ESI-MS/MS is reported. The method was optimized in terms of extraction time, buffer (ammonium formate) ratio, and graphitized carbon black (GCB) ratio for the clean-up of vegetation. The validated method yielded accuracy in terms of percentage recovery of 71–125% (soil) and 70–117% (vegetation) for the majority of 98 CUPs. The precision in terms of relative standard deviation was at 1–14% (soil), and 1–13% (vegetation). Matrix-matched calibration curves exhibited good linearities (R2 > 0.99). The limits of quantitation ranged between 0.008 and 21.5 μg kg−1 in soil and vegetation. The reported method was applied to soils and vegetation from 13 agricultural sites across Germany. Overall, 44 of the 98 common CUPs were detected in our samples and the qualitative load is well above the average for arable soils in the EU.