Analytical and Bioanalytical Chemistry

, Volume 391, Issue 4, pp 1175–1181 | Cite as

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

  • Alin C. Dirtu
  • Laurence Roosens
  • Tinne Geens
  • Adriana Gheorghe
  • Hugo Neels
  • Adrian Covaci
Original Paper
First Online:
Received:
Revised:
Accepted:

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°C). Further liquid-liquid partitioning using hexane-DCM (4:1, v/v) and K2CO3 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.

Figure

Phenolic endocrine disruptors, such as bisphenol A, triclosan and tetrabromobisphenol A, are preferentially measured in human serum at low ng/mL range.

Keywords

Bisphenol A Triclosan Tetrabromobisphenol A Solid-phase extraction Gas chromatography-mass spectrometry Human serum 
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Notes

Acknowledgments

We thank Dr Bill Lee for fruitful discussion on derivatization procedures for phenolic compounds. Dr Adrian Covaci acknowledges financial support by a postdoctoral fellowship granted by Flanders Scientific Funds for Research (FWO). Dr Adriana Gheorghe acknowledges the fellowship offered by the Francqui fonds, while Tinne Geens thanks the University of Antwerp for her scholarship. The present study was partially supported by a small project (Klein Project 2007) of the University of Antwerp offered to Adrian Covaci and was presented as poster at the Euroanalysis XIV symposium, 9–14th September 2007, Antwerp, Belgium). The authors acknowledge the thorough, but constructive, reviews of three anonymous referees.

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Copyright information

© Springer-Verlag 2007

Authors and Affiliations

  • Alin C. Dirtu
    • 1
    • 2
  • Laurence Roosens
    • 1
  • Tinne Geens
    • 1
  • Adriana Gheorghe
    • 1
    • 3
  • Hugo Neels
    • 1
  • Adrian Covaci
    • 1
  1. 1.Toxicological Centre, Department of Pharmaceutical SciencesUniversity of AntwerpWilrijkBelgium
  2. 2.Department of Inorganic and Analytical Chemistry“Al. I. Cuza” University of IassyIassyRomania
  3. 3.Department of Analytical Chemistry, Faculty of ChemistryUniversity of BucharestBucharestRomania

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