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A simple, rapid, sensitive and reproducible method based on solid-phase extraction (SPE) and acidified silica clean-up was developed for the measurement of 12 polybrominated diphenyl ethers (PBDEs), including BDE 209, and 2,2′,4,4′,5,5′-hexabromobiphenyl (BB 153) in human serum. Several solid-phase sorbents (Empore™ C₁₈, Isolute Phenyl, Isolute ENV+ and OASIS™ HLB) were tested and it was found that OASIS™ HLB (500mg) gives the highest absolute recoveries (between 64% and 95%, R.S.D.<17%, n=3) for all tested analytes and internal standards. Removal of co-extracted biogenic materials was performed using a 6ml disposable cartridge containing (from bottom to top) silica impregnated with sulphuric acid, activated silica and anhydrous sodium sulphate. PBDEs and BB 153 were quantified using a gas chromatograph coupled with a mass spectrometer (MS) operated in electron-capture …