This diploma thesis focuses on polar pesticides and their analysis in agricultural commodities. One of the aims was establishing of the method for quantitative determination of diquat and paraquat using liquid chromatography with tandem mass spectrometry. Optimization parameters based on the European reference laboratories recommendations, availability of laboratory equipment and method suitability for routine analyses were taken into account. Extraction of analytes was based on shaking with acidified methanol with formic or hydrochloric acid. Considering the matrix complexity, purification with sorbents and/or acetonitrile precipitation were applied. Method validation was carried out on several levels for selected representative agricultural commodities. Part of the thesis is a field experiment where potatoes plants were sprayed with the diquat active substance. Samples of treated plants and tubers were analyzed for diquat residues. The validated method was also used for screening of diquat and paraquat residues in feed samples collected within official controls of the Central Institute for Supervising and Testing in Agriculture in 2020. The final method enables to analyze diquat and paraquat with sensitivity suitable for the maximal residue limit controls.

Les pesticides sont aujourd’hui reconnus comme ayant des effets néfastes sur l’environnement et sur la santé humaine. La surveillance du niveau de pollution par les pesticides dans les écosystèmes aquatiques implique la mise en place d’une stratégie d’échantillonnage basée sur des prélèvements ponctuels, suivi d’une étape de traitement et d’analyse des échantillons. Par ailleurs, la concentration de ces polluants est sujette à de nombreuses fluctuations et par conséquent une faible fréquence d’échantillonnage ne donne pas une image représentative du réel niveau de pollution et de l’évolution de la qualité des masses d’eau.Ainsi, ce travail de recherche porte sur une méthode alternative d’échantillonnage basée sur l’utilisation d’échantillonneurs passifs, afin de suivre le niveau de contamination des eaux de surface et souterraines par les pesticides. Deux types d’échantillonneurs passifs, les Chemcatchers (version polaire) et les POCIS (Polar Organic Chemical Intégrative Sampler), ont été étudiés afin de comparer leurs efficacités comme outils de diagnostic et de surveillance de la pollution des milieux aquatiques par les pesticides polaires. La première phase de l’étude concerne la validation de ces outils, basée sur la calibration en laboratoire et in-situ des POCIS et des Chemcatchers, afin de permettre leurs utilisations en tant qu’outils d’analyse quantitative pour l’évaluation de la concentration moyenne des pesticides dans les masses d’eau. La deuxième partie du travail est plus orientée sur l’applicabilité de ces échantillonneurs passifs pour l’étude de la distribution spatiale des pesticides, de l’identification des sources de pollution et du transfert des polluants (eau de surface/eau souterraine). / Nowadays, pesticides are recognized as having adverse effects on the environment and human health. Monitoring the level of pesticides pollution in aquatic ecosystems involves the establishment of a sampling strategy based on a water spot sampling, followed by a stage of processing and analysis of samples. Furthermore, the concentration of these pollutants can fluctuate over time and therefore a low sampling frequency does not give a representative picture of the real level of pollution and cannot describe faithfully the changing of the quality of the water bodies.Thus, this work focuses on an alternative sampling method based on the use of passive samplers to monitor the level of contamination of surface and groundwater by pesticides. Two types of passive samplers, the polar Chemcatcher and the POCIS (Polar Organic Chemical Intégrative Sampler) were studied in order to compare the effectiveness of these tools for the diagnosis and the monitoring of aquatic pollution by polar pesticides.The first step of the study consists the validation of these two passive samplers, which is based on the laboratory and in-situ calibration of POCIS and polar Chemcatcher, to allow their use as tools for quantitative analysis for the assessment of the average concentration of pesticides in water bodies. The second part of the work is more focused on the applicability of these passive samplers for the study of the spatial distribution of pesticides, the identification of pollution sources and the assessment of pollutants transfer (surface water/groundwater).