Skip to main content
SpringerLink
Log in

Determination of ultra-trace levels of priority PBDEs in water samples by isotope dilution GC(ECNI)MS using 81Br-labelled standards

  • Original Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

A gas chromatography electron capture negative ionization mass spectrometry (GC(ECNI)MS) procedure for the determination of priority polybrominated diphenyl ethers (PBDEs; congeners 28, 47, 99, 100, 153 and 154) in water samples at regulatory EU levels has been developed. The method is based on the use of 81Br-labelled PBDEs for isotope dilution analysis and the measurement of 79Br/81Br isotope ratios in gas chromatography peaks with the electron capture negative ionization technique. The suitability of this ion source for the precise and accurate measurement of bromine isotope ratios has been demonstrated. The general ECNI-IDMS procedure was evaluated by the analysis of NIST SRM 1947 (Lake Michigan fish tissue) with satisfactory results. For the analysis of water samples, 500 mL of the samples were spiked with the labelled PBDEs and extracted with 10 mL isooctane for 30 min. The extract was evaporated down to ca. 100 μL and injected in the GC(ECNI)MS. Detection limits ranged from 0.014 −1 to 0.089 pg mL−1 depending on the congener. Recoveries from real water samples, spiked at a level of 0.5 pg mL−1, ranged from 77% to 102%.

The proposed method is based on the use of 81Br-labelled PBDE standards for isotope dilution analysis and the measurement of 79Br/81Br isotope ratios in gas chromatography peaks with the electron capture negative ionization source

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6

Similar content being viewed by others

References

  1. Rahman F, Langford KH, Scrimshaw MD, Lester JN (2001) Sci Tot Env 275:1–17

    Article  CAS  Google Scholar 

  2. U.S. Environmental Protection Agency. Polybrominated Diphenyl Ethers (PBDEs) Project Plan March 2006.

  3. Vonderheide AP, Montes-Bayón M, Caruso JAJ (2002) Anal At Spectrom 17:1480–1485

    Article  CAS  Google Scholar 

  4. Zhou J, Yang F, Cha D, Zeng Z, Xu Y (2007) Talanta 73:870–877

    Article  CAS  Google Scholar 

  5. WHO/IPCS. Environmental health criteria 162. Brominated diphenyl ethers. Geneva, Switzerland: World Health Organization

  6. Hale RC, Alaee M, Manchester-Neesvig JB, Stapleton HM, Ikonomou MG (2003) Environ Int 29:771–779

    Article  CAS  Google Scholar 

  7. Lagalante AF, Oswald TD (2008) Anal Bioanal Chem 391:2249–2256

    Article  CAS  Google Scholar 

  8. Wolkers H, Van Bavel B, Derocher AE, Wiig Ø, Kovacs KM, Lydersen C, Lindström G (2004) Environ Sci Technol 38:1667–1674

    Article  CAS  Google Scholar 

  9. Swarthout RF Jr, Kucklick JR, Davis WCJ (2008) Anal At Spectrom 23:1575–1580

    Article  CAS  Google Scholar 

  10. Domingo JLJ (2004) Chromatogr A 1054:321–326

    Article  CAS  Google Scholar 

  11. Costa LG, Giordano G, Tagliaferri S, Caglieri A, Mutti A (2008) Acta Biomed 79:172–183

    CAS  Google Scholar 

  12. Directive 2008/105/EC of the European Parliament and of the Council of 16 December 2008 on environmental quality standards in the field of water policy, amending and subsequently repealing Council Directives 82/176/EEC, 83/513/EEC, 84/156/EEC, 84/491/EEC, 86/280/EEC and amending Directive 2000/60/EC of the European Parliament and of the Council, Official Journal Of the European Communities, 24.12.2008 348:84–97

  13. European Food Safety Authority (2006) The EFSA Journal 328:1–4

    Google Scholar 

  14. Covaci A, Voorspoels S, de Boer J (2003) Environ Int 29:735–756

    Article  CAS  Google Scholar 

  15. Eljarrat E, Barceló D (2004) Trend Anal Chem 23:727–736

    Article  CAS  Google Scholar 

  16. US EPA Method 1614: Brominated Diphenyl Ethers in Waste Soil, Sediment and Tissue by HRGC/HRMS, US Environmental Protection Agency, Office of Water, Office of Science and Technology Engineering and Analysis Division, Washington, DC (2007) (EPA-821-R-07-005)

  17. Ackerman LK, Wilson GR, Simonich SL (2005) Anal Chem 77:1979–1987

    Article  CAS  Google Scholar 

  18. Peng JH, Huang CW, Weng YM, Yak HK (2007) Chemosphere 66:1990–1997

    Article  CAS  Google Scholar 

  19. Covaci A, de Boer J, Ryan JJ, Voorspoels S, Schepens P (2002) Anal Chem 74:790–798

    Article  CAS  Google Scholar 

  20. Sjödin A, Jakobsson E, Kierkegaard A, Marsh G, Sellström UJ (1998) Chromatogr A 822:83–89

    Article  Google Scholar 

  21. Stapleton HM, Keller JM, Schantz MM, Kucklick JR, Leigh SD, Wise SA (2007) Anal Bioanal Chem 387:2365–2379

    Article  CAS  Google Scholar 

  22. González-Gago A, Marchante-Gayón JM, Ferrero M, Garcia Alonso JI (2010) Anal Chem 82:2879–2887

    Article  Google Scholar 

  23. González-Gago A, Marchante-Gayón JM, Garcia Alonso JI (2011) Anal Chem 83:3024–3032

    Article  Google Scholar 

  24. De Boer J, Allchin C, Law R, Zegers B, Boon JP (2001) Trends Anal Chem 20:591–599

    Article  Google Scholar 

  25. Rodríguez-González P, Marchante-Gayón JM, García Alonso JI, Sanz-Medel A (2005) Spectrochim Acta B 60:151–207

    Article  Google Scholar 

  26. Poperechna N, Heumann KG (2005) Anal Chem 77:511–516

    Article  CAS  Google Scholar 

  27. Poperechna N, Heumann KG (2005) Anal Bioanal Chem 383:153–159

    Article  CAS  Google Scholar 

  28. Heilmann J, Heumann KG (2008) Anal Bioanal Chem 390:643–653

    Article  CAS  Google Scholar 

  29. Giese RWJ (2000) Chromatogr A 892:329–346

    Article  CAS  Google Scholar 

  30. Stemmier EA, Hites RA, Arbogast B, Budde WL, Deinzer ML, Dougherty RC, Eichelberger JW, Foltz RL, Grimm C, Grimsrud EP, Sakashita C, Sears LJ (1988) Anal Chem 60:781–787

    Article  Google Scholar 

  31. Heumann KG (1988) Isotope dilution mass spectrometry. In: Adams F, Gijbels R, Van Grieken R (eds) Inorganic mass spectrometry. Wiley, New York, pp 301–376

    Google Scholar 

  32. Böhlke JK, de Laeter JR, De Bièvre P, Hidaka H, Peiser HS, Rosman KJR, Taylor PDPJ (2005) Phys Chem Ref Data 34:57–67

    Article  Google Scholar 

  33. http://www.irmm.jrc.be/reference_materials_catalogue/user_support/Pages/index.aspx

  34. Kragten J (1994) Analyst 119:2161–2165

    Article  CAS  Google Scholar 

Download references

Acknowledgement

The work described in this paper was supported by the Ministry of Science and Innovation, Madrid, Spain (project ref. CTQ2009-12814)

Author information

Authors and Affiliations

  1. Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, 33006, Oviedo, Spain

    Adriana González-Gago, Juan Manuel Marchante-Gayón & J. Ignacio Garcia Alonso

  2. Institute for Environmental Studies, VU University, De Boelelaan 1087, 1081 HV, Amsterdam, The Netherlands

    Sicco H. Brandsma, Pim E. G. Leonards & Jacob de Boer

Authors
  1. Adriana González-Gago
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Sicco H. Brandsma
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Pim E. G. Leonards
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Jacob de Boer
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Juan Manuel Marchante-Gayón
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. J. Ignacio Garcia Alonso
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to J. Ignacio Garcia Alonso.

Electronic supplementary material

Rights and permissions

Reprints and permissions

About this article

Cite this article

González-Gago, A., Brandsma, S.H., Leonards, P.E.G. et al. Determination of ultra-trace levels of priority PBDEs in water samples by isotope dilution GC(ECNI)MS using 81Br-labelled standards. Anal Bioanal Chem 401, 2639–2649 (2011). https://doi.org/10.1007/s00216-011-5323-6

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-011-5323-6

Keywords

Search

Navigation