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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 (TM) C-18, Isolute Pheny], Isolute ENV+ and OASIS (TM) HLB) were tested and it was found that OASIS (TM) HLB (500 mg) 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 6 ml 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 negative ionization mode. The method limits of quantification (LOQ) ranged between 0.2 and 25 pg/ml serum (0. 1 and 4 ng/g lipid weight). LOQs were dependent on the analyte levels in procedural blanks which resulted in the highest LOQs for PBDE congeners found in higher concentrations in blanks (e.g. BDE 47, 99 and 209). The use of OASIS (TM) HLB SPE cartridge allowed a good method repeatability (within- and between-day precision < 12% for all congeners, except for BDE 209 < 17%, n = 3). The method was applied to serum samples from a random Belgian population. The obtained results were within the range of PBDE levels in other non-exposed population from Europe. (c) 2005 Elsevier B.V. All rights reserved.