title: Sensitive and selective method for the determination of bisphenol-A and triclosan in serum and urine as pentafluorobenzoate-derivatives using GC-ECNI/MS.
abstract: 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).
authors.affiliation: Toxicological Centre, Department of Pharmaceutical Sciences, University of Antwerp, Belgium.
authors.forename: Tinne
authors.initials: T
authors.lastname: Geens
authors.forename: Hugo
authors.initials: H
authors.lastname: Neels
authors.forename: Adrian
authors.initials: A
authors.lastname: Covaci
mesh_terms: D001559:Benzhydryl Compounds; D001565:Benzoates / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D010636:Phenols / Q000032:analysis* / Q000097:blood / Q000652:urine; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D014260:Triclosan / Q000032:analysis* / Q000097:blood / Q000652:urine; D005464:Fluorobenzenes; D005466:Fluorocarbons; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D001565:Benzoates; D010636:Phenols; D014260:Triclosan; C090819:pentafluorobenzoic acid; D005464:Fluorobenzenes; D005466:Fluorocarbons; C006780:bisphenol A; D000098826:Bisphenol A Compounds