Development of a simple multiresidue extraction method for the quantification of a wide polarity range list of pesticides and transformation products in eggs by liquid chromatography and tandem mass spectrometry

2020 
Abstract Waterfowl populations have been decreasing in Europe for the last years and pollution appears to be one of the main factors. This study was conducted to develop a single sensitive and robust analytical method for the monitoring of 2 fungicides, 15 herbicides, 3 insecticides and 24 transformation products in wild bird eggs. One of the major challenges addressed was the characterization of chemicals with large logP range (from -1.9 to 4.8). A total of 11 different extraction parameters were tested in triplicate to optimize the extraction protocol, on generic parameters, buffer addition and use of clean-up steps. Quantification was based on matrix-match approach with hen eggs as reference matrix (34 analytes with r²>0.99). Particular attention was payed to matrix effects (72 % on average), quantification limits (0.5 to 25 ng.g−1 dry mass / 0.2 to 7.5 ng.g−1 fresh mass) and extraction yields (46 to 87 % with 25 analytes up to 70 %) to ensure the relevance of the method and its compatibility with ultra-trace analysis. It led to a simple solid/liquid low temperature partitioning extraction method followed by LC-MS/MS. Analysis of 29 field samples from 3 waterfowl species revealed that eggs were slightly contaminated with pesticides as only one egg presented a contamination (terbutryn, herbicide, 0.7 ng.g−1) and confirmed the relevance of the method.
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