Method development for the analysis of polybrominated dibenzo-p-dioxins, dibenzofurans and diphenyl ethers in sediment samples

A column chromatography procedure was developed for the clean-up of solvent-extracted sediment samples for the fractionation of polybrominated diphenyl ethers (PBDEs) and polybrominated dibenzo-p-dioxins and dibenzofurans (PBDD/Fs). The procedure included multiple column chromatography steps for clean-up for the separation of PBDEs from PBDD/Fs. The separation of the two chemical groups overcame the mutual interfering problem during the GC–ion trap MS analysis. The method was validated with the analysis of quality control samples. The method accuracy represented with relative error was less than 16% for all targeted PBDEs and PBDD/Fs congeners. Recoveries of the 13C-labeled standards ranged from 64% to 117% with relative standard deviation from 7.3% to 15%. Results from the analysis of environmental sediment samples collected in the vicinity of a recycling site for electronic wastes showed high levels of PBDEs (1.5–12 ng/g, dry weight), trace levels of PBDFs (0.025–0.92 ng/g, dry weight) and non-detectable PBDDs.