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An analytical method based on headspace solid-phase microextraction gas chromatography- ion trap tandem mass spectrometry (HS-SPME-GC-ITMS/MS) was optimised and developed for estimating 20 predominant polychlorinated biphenyl (PCB) concentrations in sediment samples. The effect of experimental parameters involving fibre materials, amount of water added, temperature effect, sorption time, stirring effect, and the addition of solvents were examined with gas chromatography-electron capture detector (GC-ECD). The analytical performance of association of HS-SPME-GC-ITMS/MS proposed methodology was examined by spiked sediment with the selected PCB congeners. The repeatability and reproducibility of measurements (n = 6), expressed with relative standard deviation (RSD), was below 13% and 16%, respectively. Good linearity was observed within the concentration range studied and the LODs were between 0.02 and 0.82 ng g −1 . Accuracy was assessed by analysing a reference sediment sample with certified concentrations of several PCBs. Standard addition calibrations were done and concentrations of PCBs with the proposed method were in good agreement with the certified PCB concentrations. The method was also efficiently applied to real sample sediment from Bizerte Harbour, revealing the existence of several congeners at level less than 1.1 ng g −1 . These obtained results were also on concordance with analysis of this real sample using a conventional soxhlet extraction method. The developed procedure is highly effective and selective, free of organic solvents, relatively simple and fast, and become a suitable alternative for routine monitoring of residues of PCB from sediments at ultra-trace levels.

international journal of environmental analytical chemistry

A simple, selective and eco-friendly method for quantification of polychlorinated biphenyls in sediment samples at ultra-trace levels by headspace solid-phase microextraction-gas chromatography-ion trap tandem mass spectrometry