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The development and validation of an analytical method is presented for the determination of bisphenol-A (BPA) and triclosan (TCS), two ubiquitous contaminants, in serum and urine. The glucuronidated metabolites were first turned into their free forms to determine total BPA and TCS. The determination consisted of a solid-phase extraction on Oasis HLB cartridges followed by an extractive derivatization with pentafluorobenzoylchloride. The extract was then purified on 10% (w/w) acidified silica and analyzed by gas chromatography-mass spectrometry in electron-capture negative ionization mode. Monitored ions were m/z 616 and 406 for BPA and m/z 482 and 287 for TCS, respectively. Limits of quantification were 0.5 ng/mL in serum and 0.2 ng/mL in urine for BPA and 0.1 ng/mL in serum and 0.05 ng/mL in urine for TCS. Method recoveries were between 76 and 110%, while repeatability was below 20%. The method was applied on 20 serum and 20 urine samples. The detection frequency in serum was 10% and 55% for BPA and TCS, respectively. BPA and TCS could be detected in all urine samples with median concentrations of 1.25 ng BPA/mL (range 0.58-5.20 ng/mL) and 1.71 ng TCS/mL (0.18-672 ng/mL). (C) 2009 Elsevier B.V. All rights reserved.