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A new method for the analysis of pesticides in agricultural soils by using liquid chromatography coupled with a high-resolution quadrupole time-of-flight mass spectrometer (LC-QTOF-MS) has been developed. Twenty-four pesticides including herbicides, insecticides or fungicides have been studied. The linearity of the external calibration of the pesticides obtained from levels of concentration ranging from 0.010 to 400 µg/Lgives satisfactory results with the correlation coefficients higher than 0.99. The quantification limits of the equipment range from 0.010 to 1.250 µg/L and correspond to the lowest standard in the calibration range for which the residual deviation is less than 60%. An experimental design has been used to optimise the parameters of pressurised-liquid extraction (PLE) of pesticides in soils. The optimised conditions have been found by using methanol as extraction solvent at a temperature of 80°C, a pressure of 150 Bars and 2 extraction cycles of 5 minutes. The mean recoveries of pesticides (Mean) are higher than 72% with a relative standard deviation(RSD) less than 21%. These results demonstrate the good efficiency of PLE for the extraction of pesticides in agricultural soils of different nature. The LC-QTOF-MS is a sensitive, linear and robust instrument for the quantification of pesticides in unpurified soil extracts by external calibration. This analytical tool is not subjected to matrix effects of soil extracts.

international journal of environmental analytical chemistry

A new, simple, efficient and robust multi-residue method based on pressurised-liquid extraction of agricultural soils to analyze pesticides by liquid chromatography coupled with a high resolution quadrupole time-of-flight mass spectrometer