title: Simultaneous determination of bisphenol A, triclosan, and tetrabromobisphenol A in human serum using solid-phase extraction and gas chromatography-electron capture negative-ionization mass spectrometry.
abstract: This study aimed at optimizing and validating a sensitive method for simultaneous determination of bisphenol A (BPA), triclosan (TCS), and tetrabromobisphenol A (TBBPA) in human serum using solid-phase extraction (SPE) and gas chromatography coupled to electron-capture negative-ionization mass spectrometry (GC-ECNI/MS). Sample preparation involved denaturation of serum proteins with formic acid followed by SPE on an Oasis HLB cartridge. Fractionation was performed on Florisil from which the phenolic compounds were eluted with methanol-dichloromethane (DCM) (5:1, v/v). The phenolic fraction was further derivatized with pentafluoropropionic acid anhydride (30 min at 70 degrees C). Further liquid-liquid partitioning using hexane-DCM (4:1, v/v) and K(2)CO(3) 3% aqueous solution was used to eliminate excess reagent and acidic by-products formed during derivatization. The cleaned extract was injected into a GC-ECNI/MS system operated in selected ion monitoring mode. For thorough method validation, each step of the procedure was rigorously optimized. The method limits of quantitation for BPA, TCS, and TBBPA were 0.28 ng mL(-1), 0.09 ng mL(-1) and 0.05 ng mL(-1), respectively. Furthermore, the method was applied to 21 Belgian human serum samples. The median concentrations obtained for BPA (0.71 ng mL(-1)) and TCS (0.52 ng mL(-1)) in Belgian human serum samples were similar to previously reported data for human fluids. Slightly higher levels of TBBPA (0.08 ng mL(-1)) were found in Belgium samples compared to Norwegian serum.
authors.affiliation: Toxicological Centre, Department of Pharmaceutical Sciences, University of Antwerp, Universiteitsplein 1, 2610, Wilrijk, Belgium.
authors.forename: Alin C
authors.initials: AC
authors.lastname: Dirtu
authors.forename: Laurence
authors.initials: L
authors.lastname: Roosens
authors.forename: Tinne
authors.initials: T
authors.lastname: Geens
authors.forename: Adriana
authors.initials: A
authors.lastname: Gheorghe
authors.forename: Hugo
authors.initials: H
authors.lastname: Neels
authors.forename: Adrian
authors.initials: A
authors.lastname: Covaci
mesh_terms: D000328:Adult; D001559:Benzhydryl Compounds; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation* / Q000379:methods*; D006801:Humans; D008297:Male; D008875:Middle Aged; D015394:Molecular Structure; D010636:Phenols / Q000097:blood* / Q000737:chemistry; D011075:Polybrominated Biphenyls / Q000097:blood* / Q000737:chemistry; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000295:instrumentation / Q000379:methods*; D014260:Triclosan / Q000097:blood* / Q000737:chemistry; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D010636:Phenols; D011075:Polybrominated Biphenyls; D014260:Triclosan; C020806:tetrabromobisphenol A; C006780:bisphenol A; D000098826:Bisphenol A Compounds