Rapid multiresidue determination of organochlorine and organophosphorus compounds in human serum by solid-phase extraction and gas chromatography coupled to tandem mass spectrometry

A rapid analytical method for the multiresidue determination of several organochlorine and organophosphorus pesticides and polychlorinated biphenyls in human serum samples has been developed. Analytes were isolated by solid-phase extraction using C18 cartridges with subsequent analysis by GC-MS/MS using a glass liner packed with CarboFrit in the GC injection port. Labelled surrogate internal standards (fenitrothion D6, HCB (13)C6, p,p'-DDE D8 and PCB 13 8 (13)C12) were added to the samples before the extraction and were used for quantitation and for quality control in the analysis of real-world samples. Accuracy and precision were evaluated by using serum samples fortified at two concentration levels for the three families of compounds, with satisfactory results in the majority of cases. The high selectivity and sensitivity of GC-MS/MS allowed low detection limits of 0.05-0.5 ng mL(-1) for most of the analytes investigated. The developed procedure improves other current methodologies for the analysis of pesticides and PCBs in biological fluids, especially as regards to analysis time and simplicity of sample treatment. The method was applied to several serum samples obtained from farmers devoted to citrus crop production. Chlorpyrifos, HCB, p,p'-DDE and the higher chlorinated PCBs (153, 138 and 180) were the most frequently detected compounds.