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A fast extraction and clean-up method for the simultaneous determination of PCBs and PBDEs has been developed. The procedure consisted of a solid-phase extraction (SPE) of the analytes on an Oasis (R) HLB cartridge and the subsequent on-line fat elimination by directly dropping the eluate from the SPE cartridge onto a second cartridge containing layers of activated neutral silica gel and sulphuric acid modified silica gel. Detection limits using a gas chromatography coupled with an ion trap detector in the tandem mass spectrometry mode were from 0.03 to 0.3 pg/mu L for PCBs and from 0.07 to 1.3 pg/mu L for PBDEs. Repeatability (lower than I I %) and reproducibility (lower than 17%), expressed as relative standard deviation (RSD, n = 4), were satisfactory. The feasibility of the method developed for the determination of the target compounds was evaluated by participation in several rounds of interlaboratory exercises involving human serum with a wide range of PBDE and PCB concentrations. The method has been applied to the evaluation of PBDEs and PCBs in human serum samples of up to 1 mL. (C) 2006 Elsevier B.V. All rights reserved.