Miniaturized multiresidue method for the analysis of pesticides and persistent organic pollutants in non-target wildlife animal liver tissues using GC-MS/MS

Abstract

In order to gain a better insight into pesticide and pollutant exposure of small (non-target) wildlife animals, a QuEChERS sample preparation method was first developed for 5 g liver tissues (e.g. hedgehog samples) and then downscaled for the analysis of 100 mg liver tissues (e.g. bat samples). The optimized (micro) QuEChERS methods used 1% acetic acid in acetonitrile as organic solvent for liquid-liquid extraction (LLE) and salting out was performed with anhydrous magnesium sulfate and sodium acetate (4:1). After a freezing-out step, sample clean-up was carried out with anhydrous magnesium sulfate, PSA, C18, and GCB (150:25:20:5). Overall, 209 pesticides and persistent organic pollutants (POPs) can be analysed within each sample with gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Both methods were validated with representative analytes according to the European Commission guideline SANTE/12682/2019. Limits of quantification were between 1 and 20 μg kg−1, and the methods proved to be linear up to 400 μg kg−1. Additionally, the analytes delivered satisfactory results regarding recovery and precision. As proof of concept, samples of six hedgehog livers were analysed with both methods to prove the accuracy of the micro QuEChERS method. Additionally, six livers of different bat species were analysed with the downscaled method. The newly developed micro QuEChERS method for multiresidue analysis requires only minute amounts of biomaterial and represents a sophisticated novel technique for determining the exposure of small wildlife animals to different contaminants.