Determination of multi pesticide residues in leaf and needle samples using a modified QuEChERS approach and gas chromatography-tandem mass spectrometry

Abstract

In order to gain a better insight into pesticide and pollutant exposure in forests, a rapid and sensitive gas chromatography-tandem mass spectrometry (GC-MS/MS) method for the determination of 208 pesticide residues in leaves and needles has been established. The modified QuEChERS (quick, easy, cheap, effective, rugged and safe) approach uses 2 g of homogenized sample, acetonitrile and water as extraction agents, combined with citrate buffer for the following salting out step. The limits of quantification (LOQs) were determined to 0.0025–0.05 mg kg⁻¹, respectively. Calibration curves showed a linear range between the respective LOQ and 1.0 mg kg⁻¹ with coefficients of determination (R²) ≥ 0.99 for all analyzed pesticides. The recovery rates ranged from 69.7% to 92.0% with a relative standard deviation below 20%. The analysis of beech leaves, spruce and pine needles (each n = 3) provided a proof of concept for the developed methodology and revealed the presence of six pesticide residues (boscalid, epoxiconazole, fenpropimorph, lindane, terbuthylazine, terbuthylazine-desethyl). The results underline the strong need for systematic surveillance of the uncontrollable exposure of pesticides to nature.