Multitargeted analysis for the simultaneous determination of organochlorine pesticides and polychlorinated biphenyls in sediments exploiting comprehensive two-dimensional gas chromatography coupled to mass spectrometry

Persistent organic pollutants (POPs), including organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs), remain a significant environmental concern due to their persistence, bioaccumulation, and toxicity. Accurate quantification of these contaminants in sediment matrices remains analytically challenging due to the complexity of the matrix and the need for detection at trace levels to meet regulatory standards. This research focused on the development and application of an analytical protocol for the simultaneous determination of OCPs and PCBs in sediments using solid-phase extraction (SPE) followed by comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS). The developed method was validated, achieving low limits of detection (0.4 to 14 ng kg-1) and quantification (1.1 to 41 ng kg-1), with satisfactory linearity (r² > 0.99), accuracy (90–110%), and precision (RSD < 5%) for all target analytes. Validation with certified reference material confirmed the agreement between experimental and certified concentrations for most compounds. The protocol was applied to environmental sediment samples, detecting multiple PCBs and DDT-related compounds at concentrations below international guideline values. These results confirm the method's suitability for trace-level determination of OCPs and PCBs in sediments, addressing the analytical demands of environmental monitoring and regulatory compliance. The established protocol enables sensitive and reliable assessment of sediment contamination, supporting a simultaneous ongoing surveillance and risk assessment of such classes of persistent organic pollutants in the same analytical run.