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.