Development of a Dispersive µSPE Method for the Determination of Pesticide Residues in Water Samples by LC-MS/MS

The increasing occurrence of pesticides in aquatic environments has raised concern due to their potential impact on human health and ecosystems. In this context, the development of sensitive, reliable, and environmentally sustainable analytical methods is essential for monitoring these contaminants. Therefore, the aim of this study was to develop and validate a miniaturized dispersive solid-phase extraction (DµSPE) method for the determination of current-use multiclass pesticides in water samples using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Initially, a simple and rapid sample preparation procedure was developed, in which different experimental variables were evaluated to obtain suitable extraction efficiency. The validated method has a quantification limit of 0.01 µg L−1 and was applied to the determination of pesticides in surface water from different regions in Rio Grande do Sul State, Brazil. In addition, the environmental sustainability of the method was evaluated using the AGREEprep tool, allowing a quantitative and visual assessment of its compliance with the principles of Green Analytical Chemistry. The results demonstrated that the proposed method provides adequate analytical performance for the determination of 28 compounds in water matrices while offering a simple sample preparation procedure with reduced solvent consumption and waste generation.