Optimization and validation of a QuEChERS-based method for the simultaneous environmental monitoring of 218 pesticide residues in clay loam soil

Abstract

A modified QuEChERS method was optimized, validated and verified for the extraction of 218 pesticide residues in agricultural soil samples. The 218 analytes are extracted using a single step, without clean-up, with matrix-matched calibration, and two complementary techniques: liquid and gas chromatography tandem triple quad mass spectrometry (LC-MS/MS and GC-MS/MS). Some of the parameters such as salts, acidity of the extraction solvent, sample moisture and some mechanical changes in the procedure were optimized to improve the overall performance for the target compounds and the soil matrix. The method was fully validated on a representative agricultural soil sample of the Canary Islands (clay loam soil) in terms of linearity, accuracy and precision. To avoid matrix effects, matrix-matched calibration curves (R² ≥ 0.99) were used for all target analytes. 100% of the compounds can be quantified with limits of quantification (LOQ) lower than the limit typically used in soils (50 ng g^-1), with 92% of compounds presenting a LOQ that is at least 10 times lower than that normally required. The limits of detection (LOD) ranged between 0.024 and 6.25 ng g^-1. The validated method was applied to a series of actual samples of agricultural soil (n = 18). In addition, as a further verification of its potential, the results of the application of the method in the investigation of clay loam soil samples that were obtained from underneath wildlife carcasses in the context of an environmental forensic investigation are also presented.

Keywords: GC–MS/MS; LC-MS/MS; Multi-residue extraction method; Pesticides; QuEChERS; Soils.