Analytical and Bioanalytical Chemistry

, Volume 391, Issue 6, pp 2249–2256 | Cite as

Analysis of polybrominated diphenyl ethers (PBDEs) by liquid chromatography with negative-ion atmospheric pressure photoionization tandem mass spectrometry (LC/NI-APPI/MS/MS): application to house dust

Original Paper

Abstract

Eight polybrominated diphenyl ether (PBDE) congeners of primary interest to the US EPA were separated using reverse-phase liquid chromatography on an octadecylsilane column. BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, BDE-183, and BDE-209 were baseline-resolved under isocratic conditions in 92:8 methanol/water (v/v). Negative-ion atmospheric pressure photoionization (NI-APPI) with a toluene dopant produced precursor ions corresponding to [M–Br+O] for the eight congeners studied. Each congener was quantified by tandem mass spectrometry through a unique multiple reaction monitoring (MRM) transition. On-column limits of detection were between 2.4 and 27.8 pg for the eight congeners studied, with an intra-day method precision of 9%. The LC/NI-APPI/MS/MS method was validated for the analysis of the eight PBDE congeners in NIST SRM 2585 (Organics in House Dust). Pressurized liquid extraction (PLE) with subsequent LC/NI-APPI/MS/MS analysis afforded quantitative recovery for all eight PBDE congeners with recoveries ranging from 92.7 to 113%. The liquid-phase separation of the LC/NI-APPI/MS/MS method is not prone to the thermal degradation issues that plague splitless GC based analyses of highly brominated PBDEs such as BDE-209.

Keywords

Negative-ion atmospheric pressure photoionization (NI-APPI) Liquid chromatography tandem mass spectrometry (LC/MS/MS) Dust Polybrominated diphenyl ethers (PBDEs) Pressurized liquid extraction (PLE) 

References

  1. 1.
    La Guardia MJ, Hale RC, Harvey E (2006) Environ Sci Technol 40:6267–6254CrossRefGoogle Scholar
  2. 2.
    Sjödin A, Jokobsson E, Kierkegaard A, Marsh G, Sellström U (1998) J Chromatogr A 822:83–89CrossRefGoogle Scholar
  3. 3.
    Hale RC, La Guardia MJ, Harvey E, Mainor TM (2002) Chemosphere 46:729–735CrossRefGoogle Scholar
  4. 4.
    Renner R (2004) Environ Sci Technol 38:14AGoogle Scholar
  5. 5.
    BSEF (2001) Major brominated flame retardants volume estimates. Bromine Science and Environmental Forum, Brussels (see http://www.bsef.com/docs/BFR_vols_2001.doc, last accessed 28 April 2008)
  6. 6.
    Stapleton H, Letcher R, Baker J (2002) Organohal Compd 58:201–204Google Scholar
  7. 7.
    Alaee M, Wenning RJ (2002) Chemosphere 46:579–796CrossRefGoogle Scholar
  8. 8.
    de Wit CA (2002) Chemosphere 46:583–624CrossRefGoogle Scholar
  9. 9.
    Lectcher R, Behnisch P (2003) Environ Int 29:663–885CrossRefGoogle Scholar
  10. 10.
    Benedict RT, Stapleton HM, Letcher RJ, Mitchelmore CL (2007) Chemosphere 69:987–993CrossRefGoogle Scholar
  11. 11.
    Betts KS (2004) Environ Sci Technol 38:50A–51ACrossRefGoogle Scholar
  12. 12.
    Gouin T, Harner T, Daly GL, Wania F, Mackay D, Jones KC (2005) Atmos Environ Part A 39:151–166Google Scholar
  13. 13.
    Mazdai A, Dodder NG, Abernathy MP, Hites RA, Bigsby RM (2003) Environ Health Perspect 111:1249–1252Google Scholar
  14. 14.
    Petreas M, She J, Brown R, Winkler J, Winham G, Rogers E, Zhao G, Bhatia R, Charles MJ (2003) Environ Health Perspect 111:1175–1179Google Scholar
  15. 15.
    Sellström U, De Wit CA, Lundgren N, Tysklind M (2005) Environ Sci Technol 39:9064–9070CrossRefGoogle Scholar
  16. 16.
    Thuresson K, Höglund P, Hagmar L, Sjödin A, Bergman A, Jakobsson E (2006) Environ Health Perspect 114:176–181Google Scholar
  17. 17.
    Bocio A, Llobet JM, Domingo JL, Corbella J, Teixidó A, Casas C (2003) J Agric Food Chem 51:3191–3195CrossRefGoogle Scholar
  18. 18.
    Schecter AN, Päpke O, Harris RT, Tung KC, Musumba A, Olson J, Birnbaum L (2006) Environ Health Perspect 114:1515–1520CrossRefGoogle Scholar
  19. 19.
    Schecter A, Päpke O, Tung K, Staskal D, Birnbaum L (2004) Environ Sci Technol 38:5306–5311CrossRefGoogle Scholar
  20. 20.
    Allen JG, McClean MD, Stapleton HM, Nelson JW, Webster TF (2007) Environ Sci Technol 41:4574–4579CrossRefGoogle Scholar
  21. 21.
    Stapleton HM, Dodder NG, Offenberg JH, Schantz MM, Wise SA (2005) Environ Sci Technol 39:925–931CrossRefGoogle Scholar
  22. 22.
    Jones-Otazo HA, Clarke JP, Diamond ML, Archbold JA, Ferguson G, Harner T, Richardson GM, Ryan JJ, Wilford B (2005) Environ Sci Technol 39:5121–5530CrossRefGoogle Scholar
  23. 23.
    Stapleton HM, Harner T, Shoeib M, Keller JM, Schantz MM, Leigh SD, Wise SA (2006) Anal Bioanal Chem 384:791–800CrossRefGoogle Scholar
  24. 24.
    Harrad S, Hazrati S, Ibarra C (2006) Environ Sci Technol 40:4633–4638CrossRefGoogle Scholar
  25. 25.
    Tan J, Cheng SM, Loganath A, Chong YS, Obbard JP (2007) Chemosphere 66:985–992CrossRefGoogle Scholar
  26. 26.
    Karlsson M, Julander A, van Bavel B, Hardel L (2007) Environ Int 33:62–69CrossRefGoogle Scholar
  27. 27.
    Wu N, Herrmann T, Paepke O, Tickner J, Hale R, Harvey E, La Guardia MJ, McClean MD, Webster TF (2007) Environ Sci Technol 41:1584–1589CrossRefGoogle Scholar
  28. 28.
    Schecter A, Päpke O, Joseph JE, Tung K (2005) J Toxicol Environ Health 68:501–513CrossRefGoogle Scholar
  29. 29.
    Tulve NS, Suggs JC, McCurdy T, Cohen Hubal EA, Moya J (2002) J Expo Anal Environ Epidemiol 12:259–264CrossRefGoogle Scholar
  30. 30.
    Covaci A, Voorspoels S, Ramos L, Neels H, Blust R (2007) J Chromatogr A 1153:145–171CrossRefGoogle Scholar
  31. 31.
    Stapleton HM (2006) Anal Bioanal Chem 386:807–817CrossRefGoogle Scholar
  32. 32.
    Björklund J, Tollbäck P, Östman C (2003) J Mass Spectrom 38:394–400CrossRefGoogle Scholar
  33. 33.
    Ackerman LK, Wilson GR, Simonich SL (2007) Anal Chem 77:1979–1987CrossRefGoogle Scholar
  34. 34.
    Regueiro J, Llompart M, Garcia-Jares C, Cela R (2007) Anal Bioanal Chem 388:1095–1107CrossRefGoogle Scholar
  35. 35.
    Björklund J, Tollbäck P, Hiärne C, Dyremark E, Östman C (2004) J Chromatogr A 1041:201–210CrossRefGoogle Scholar
  36. 36.
    Rogers E, Petreas M, Park J, Zhao G, Charles MJ (2004) J Chromatogr B 813:269–285CrossRefGoogle Scholar
  37. 37.
    Covaci A, de Boer J, Ryan JJ, Voorspoels S, Schepens P (2002) Anal Chem 74:790–798CrossRefGoogle Scholar
  38. 38.
    Worall K, Newton A, Van Bavel B, Pettersson A, Linstrom G, Reiner E, Macpherson K, Kolic T, Ordsmith N, Catterall S (2004) Organohalog Compd 66:186–190Google Scholar
  39. 39.
    Schummler M, Brandl F, Mäurer A, van Eldik R (2005) J Chromatogr A 1064:39–51CrossRefGoogle Scholar
  40. 40.
    Pohlein M, Llopis AS, Wolf M, Van Eldik R (2005) J Chromatogr A 1066:111–117CrossRefGoogle Scholar
  41. 41.
    Debrauwer L, Riu A, Jouahri M, Rathahao E, Jouanin I, Antignac J, Cariou R, Le Bizec B, Zalko D (2005) J Chromatogr A 1082:98–109CrossRefGoogle Scholar
  42. 42.
    Cariou R, Antignac J, Debrauwer L, Maume D, Fabrice M, Zalko D, Le Bizec B, Andre F (2006) J Chromatogr Sci 44:489–497Google Scholar
  43. 43.
    Basso E, Marotta E, Seraglia R, Tubaro M, Traldi P (2003) J Mass Spectrom 38:1113–1115CrossRefGoogle Scholar
  44. 44.
    Riu A, Zalko D, Debrauwer L (2006) Rapid Commun Mass Spectrom 20:2133–2142CrossRefGoogle Scholar
  45. 45.
    Short LC, Cai S, Syage JA (2007) J Am Soc Mass Spectrom 18:589–599CrossRefGoogle Scholar
  46. 46.
    Robb DB, Blades MW (2005) J Am Soc Mass Spectrom 16:1275–1290CrossRefGoogle Scholar
  47. 47.
    Kauppila TJ, Kotiaho T, Kostiainen R, Bruins AP (2004) J Am Soc Mass Spectrom 15:203–211CrossRefGoogle Scholar
  48. 48.
    Gómara B, Herrero L, González MJ (2007) Anal Chim Acta 597:121–128CrossRefGoogle Scholar
  49. 49.
    Stapleton H, Keller JM, Schantz MM, Kucklick JR, Leigh SD, Wise SA (2007) Anal Bioanal Chem 387:2365–2379CrossRefGoogle Scholar
  50. 50.
    De Boer J, Cofino WP (2002) Chemosphere 46:625–633CrossRefGoogle Scholar
  51. 51.
    Thomsen C, Leknes H, Lundanes E, Becher G (2001) J Chromatogr A 923:299–304CrossRefGoogle Scholar

Copyright information

© Springer-Verlag 2008

Authors and Affiliations

  1. 1.Department of ChemistryVillanova UniversityVillanovaUSA

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