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.
Similar content being viewed by others
References
Staples CA, Dorn PhB, Klecka GM, O’Block ST, Harris LR (1998) Chemosphere 36:2149–2173
Vandenberg LN, Hauser R, Marcus M, Olea N, Welshons WV (2007) Reprod Toxicol 24:139–177
Vom Saal FS, Hughes C (2005) Environ Health Perspect 113:926–933
Kang JH, Kondo F, Katayama Y (2006) Toxicology 226:79–89
Bhargava HN, Leonard PA (1996) Am J Infect Control 24:209–218
Perencevich EN, Wong MT, Harris AD (2001) Am J Infect Control 28:281–283
Adolfsson-Erici M, Petterson M, Parkkonen J, Sturve J (2002) Chemosphere 46:1485–1489
Environment Health Criteria 172 (1995) Tetrabromobisphenol A and derivatives. International Program on Chemical Safety, World Health Organization, Geneva, Switzerland
Peck AM (2006) Anal Bioanal Chem 386:907–939
Tan BLL, Hawker DW, Müller JF, Leusch FDL, Tremblay LA, Chapman HF (2007) Environ Int 33:654–669
Lee HB, Peart TE, Gris G, Chan J (2002) Water Qual Res J Canada 37:459–472
Lee HB, Peart TE (2002) Qual Res J Canada 37:681–696
Heidler J, Halden RU (2007) Chemosphere 66:362–369
Shintani H (2001) Chromatographia 53:331–333
Zhang J, Jiang M, Zou L, Shi D, Mei S, Zhu Y, Shi Y, Dai K, Lu B (2006) Anal Bioanal Chem 385:780–786
Kuruto-Niwa R, Tateoka Y, Usuki Y, Nozawa R (2007) Chemosphere 66:1160–1164
Inoue K, Yoshida S, Nakayama S, Ito R, Okanouchi N, Nakazawa H (2006) Arch Environ Contam Toxicol 51:503–508
Brossa L, Pocurull E, Borrull F, Marcé RM (2004) Chromatographia 59:419–423
Zhang ZL, Hibberd A, Zhou JL (2006) Anal Chim Acta 577:52–61
Loos R, Hanke G, Eisenreich SJ (2003) J Environ Monit 5:384–394
Jeannot R, Sabik H, Sauvard E, Dagnak T, Dohrendorf K (2002) J Chromatogr A 974:143–159
Allmyr M, McLachlan MS, Sandborgh-Englund G, Adolfsson-Erici M (2006) Anal Chem 78:6542–6546
Liu R, Zhou JL, Wilding A (2004) J Chromatogr A 1022:179–189
Gatidou G, Thomaidis NS, Stasinakis AS, Lekkas TD (2007) J Chromatogr A 1138:32–41
Yoshimura Y, Brock JW, Makino T, Nakazawa H (2002) Anal Chim Acta 458:331–336
Xiao Q, Li Y, Ouyang H, Xu P, Wu D (2006) J Chromatogr B 830:322–329
Sandborgh-Englund G, Adolfsson-Erici M, Odham G, Ekstrand J (2006) J Toxicol Environ Health 69:1861–1873
Sun Y, Irie M, Kishikawa N, Wada M, Kuroda N, Nakashima K (2004) Biomed Chromatogr 18:501–507
Kuroda N, Kinoshita Y, Sun Y, Wada M, Kishikawa N, Nakashima K, Makino T, Nakazawa H (2003) J Pharm Biomed 30:1743–1749
Ye X, Kuklenyik Z, Needham LL, Calafat AM (2006) J Chromatogr B 831:110–115
Sajiki J, Takahashi K, Yonekubo J (1999) J Chromatogr B 736:255–261
Schönfelder G, Wittfoht W, Hopp H, Talsness CE, Paul M, Chahoud I (2002) Environ Health Perspect 110:A703–A707
Allmyr M, Adolfsson-Erici M, McLachlan M, Sandborgh-Englund G (2006) Sci Total Environ 372:87–93
Thomsen C, Liane VH, Becher G (2007) J Chromatogr B 846:252–263
Cariou R, Antignac JP, Marchand P, Berrebi A, Zalko D, Andre F, Le Bizec B (2005) J Chromatogr A 1100:144–152
Jakobsson K, Thuresson K, Rylander L, Sjödin A, Hagmar L, Bergman Å (2002) Chemosphere 46:709–716
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.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Dirtu, A.C., Roosens, L., Geens, T. et al. 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. Anal Bioanal Chem 391, 1175–1181 (2008). https://doi.org/10.1007/s00216-007-1807-9
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00216-007-1807-9