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Determination of perfluorinated alkyl acid concentrations in biological standard reference materials

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Abstract

Standard reference materials (SRMs) are homogeneous, well-characterized materials used to validate measurements and improve the quality of analytical data. The National Institute of Standards and Technology (NIST) has a wide range of SRMs that have mass fraction values assigned for legacy pollutants. These SRMs can also serve as test materials for method development, method validation, and measurement for contaminants of emerging concern. Because inter-laboratory comparison studies have revealed substantial variability of measurements of perfluoroalkyl acids (PFAAs), future analytical measurements will benefit from determination of consensus values for PFAAs in SRMs to provide a means to demonstrate method-specific performance. To that end, NIST, in collaboration with other groups, has been measuring concentrations of PFAAs in a variety of SRMs. Here we report levels of PFAAs and perfluorooctane sulfonamide (PFOSA) determined in four biological SRMs: fish tissue (SRM 1946 Lake Superior Fish Tissue, SRM 1947 Lake Michigan Fish Tissue), bovine liver (SRM 1577c), and mussel tissue (SRM 2974a). We also report concentrations for three in-house quality-control materials: beluga whale liver, pygmy sperm whale liver, and white-sided dolphin liver. Measurements in SRMs show an array of PFAAs, with perfluorooctane sulfonate (PFOS) being the most frequently detected. Reference and information values are reported for PFAAs measured in these biological SRMs.

NIST SRMs 1946 Lake Superior Fish Tissue and 1947 Lake Michigan Fish Tissue

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References

  1. Paul AG, Jones KC, Sweetman AJ (2009) A first global production, emission, and environmental inventory for perfluorooctane sulfonate. Environ Sci Technol 43:386–392

    Article  CAS  Google Scholar 

  2. Prevedouros K, Cousins IT, Buck RC, Korzeniowski SH (2006) Sources, fate and transport of perfluorocarboxylates. Environ Sci Technol 40:32–44

    Article  CAS  Google Scholar 

  3. Kannan K, Koistinen J, Beckmen K, Evans T, Gorzelany JF, Hansen KJ, Jones PD, Helle E, Nyman M, Giesy JP (2001) Accumulation of perfluorooctane sulfonate in marine mammals. Environ Sci Technol 35:1593–1598

    Article  CAS  Google Scholar 

  4. Kannan K, Franson JC, Bowerman WW, Hansen KJ, Jones PD, Giesy JP (2001) Perfluorooctane sulfonate in fish-eating water birds including bald eagles and albatrosses. Environ Sci Technol 35:3065–3070

    Article  CAS  Google Scholar 

  5. Moody CA, Martin JW, Kwan WC, Muir DCG, Mabury SA (2002) Monitoring perfluorinated surfactants in biota and surface water samples following an accidental release of fire-fighting foam into Etobicoke Creek. Environ Sci Technol 36:545–551

    Article  CAS  Google Scholar 

  6. Martin JW, Whittle DM, Muir DC, Mabury SA (2004) Perfluoroalkyl contaminants in a food web from Lake Ontario. Environ Sci Technol 38:5379–5385

    Article  CAS  Google Scholar 

  7. Tomy GT, Budakowski W, Halldorson T, Helm PA, Stern GA, Friesen K, Pepper K, Tittlemier SA, Fisk AT (2004) Fluorinated organic compounds in an eastern Arctic marine food web. Environ Sci Technol 38:6475–6481

    Article  CAS  Google Scholar 

  8. Houde M, Martin JW, Letcher RJ, Solomon KR, Muir DC (2006) Biological monitoring of polyfluoroalkyl substances: a review. Environ Sci Technol 40:3463–3473

    Article  CAS  Google Scholar 

  9. Chen CL, Lu YL, Zhang X, Geng J, Wang TY, Shi YJ, Hu WY, Li J (2009) A review of spatial and temporal assessment of PFOS and PFOA contamination in China. Chem Ecol 25:163–177

    Article  CAS  Google Scholar 

  10. Fujii S, Polprasert C, Tanaka S, Lien NPH, Qiu Y (2007) New POPs in the water environment: distribution, bioaccumulation and treatment of perfluorinated compounds—a review paper. J Water Supply Res Technol 56:313–326

    Article  CAS  Google Scholar 

  11. van Leeuwen SPJ, Swart CP, van der Veen I, de Boer J (2009) Significant improvements in the analysis of perfluorinated compounds in water and fish: results from an interlaboratory method evaluation study. J Chromatogr A 1216:401–409

    Article  Google Scholar 

  12. Van Leeuwen SPJ, Karrman A, Van Bavel B, De Boer J, Lindstrom G (2006) Struggle for quality in determination of perfluorinated contaminants in environmental and human samples. Environ Sci Technol 40:7854–7860

    Article  Google Scholar 

  13. Lindstrom G, Karrman A, van Bavel B (2009) Accuracy and precision in the determination of perfluorinated chemicals in human blood verified by interlaboratory comparisons. J Chromatogr A 1216:394–400

    Article  Google Scholar 

  14. Keller JM, Calafat AM, Kato K, Ellefson ME, Reagen WK, Strynar M, O'Connell S, Butt CM, Mabury SA, Small J, Muir DCG, Leigh SD, Schantz MM (2010) Determination of perfluorinated alkyl acid concentrations in human serum and milk standard reference materials. Anal Bioanal Chem 397:439–451

    Article  CAS  Google Scholar 

  15. Riddell N, Arsenault G, Benskin JP, Chittim B, Martin JW, McAlees A, McCrindle R (2009) Branched perfluorooctane sulfonate isomer quantification and characterization in blood serum samples by HPLC/ESI-MS(/MS). Environ Sci Technol 43:7902–7908

    Article  CAS  Google Scholar 

  16. Wise SA, Poster DL, Kucklick JR, Keller JM, Vanderpol SS, Sander LC, Schantz MM (2006) Standard reference materials (SRMs) for determination of organic contaminants in environmental samples. Anal Bioanal Chem 386:1153–1190

    Article  CAS  Google Scholar 

  17. Reiner JL, Phinney KW, Keller JM (2011) Determination of perfluorinated compounds in human plasma and serum Standard Reference Materials using independent analytical methods. Anal Bioanal Chem 401:2899–2907

    Article  CAS  Google Scholar 

  18. Reagen WK, Ellefson ME, Kannan K, Giesy JP (2008) Comparison of extraction and quantification methods of perfluorinated compounds in human plasma, serum, and whole blood. Anal Chim Acta 628:214–221

    Article  CAS  Google Scholar 

  19. Benskin JP, Bataineh M, Martin JW (2007) Simultaneous characterization of perfluoroalkyl carboxylate, sulfonate, and sulfonamide isomers by liquid chromatography-tandem mass spectrometry. Anal Chem 79:6455–6464

    Article  CAS  Google Scholar 

  20. DerSimonian R, Laird N (1986) Meta-analysis in clinical trials. Control Clin Trials 7:177–188

    Article  CAS  Google Scholar 

  21. Rukhin A (2009) Metrologia 46:323–331

    Article  Google Scholar 

  22. Horn RA, Horn SA, Duncan DB (1975) Estimating hetroscedastic variance in linear models. J Am Stat Assoc 70:380–385

    Article  Google Scholar 

  23. Metrology JCfGi (2008) Evaluation of measurement data—guide to the expression of uncertainty in measurement (ISO GUM 1995 with minor corrections)

  24. Metrology JCfGi (2008) Evaluation of measurement data—supplement 1 to the guide to expression of uncertainty in measurement; propagation of distributions using a Monte Carlo method

  25. Butt CM, Berger U, Bossi R, Tomy GT (2010) Levels and trends of poly- and perfluorinated compounds in the arctic environment. Sci Total Environ 408:2936–2965

    Article  CAS  Google Scholar 

  26. Delinsky AD, Strynar MJ, Nakayama SF, Varns JL, Ye X, McCann PJ, Lindstrom AB (2009) Determination of ten perfluorinated compounds in bluegill sunfish (Lepomis macrochirus) fillets. Environ Res 109:975–984

    Article  CAS  Google Scholar 

  27. Hoff PT, Van Campenhout K, de Vijver K, Covaci A, Bervoets L, Moens L, Huyskens G, Goemans G, Belpaire C, Blust R, De Coen W (2005) Perfluorooctane sulfonic acid and organohalogen pollutants in liver of three freshwater fish species in Flanders (Belgium): relationships with biochemical and organismal effects. Environ Pollut 137:324–333

    Article  CAS  Google Scholar 

  28. Furdui VI, Stock NL, Ellis DA, Butt CM, Whittle DM, Crozier PW, Reiner EJ, Muir DC, Mabury SA (2007) Spatial distribution of perfluoroalkyl contaminants in lake trout from the Great Lakes. Environ Sci Technol 41:1554–1559

    Article  CAS  Google Scholar 

  29. Delinsky AD, Strynar MJ, McCann PJ, Varns JL, McMillan L, Nakayama SF, Lindstrom AB (2010) Geographical distribution of perfluorinated compounds in fish from Minnesota lakes and rivers. Environ Sci Technol 44:2549–2554

    Article  CAS  Google Scholar 

  30. Tomy GT, Pleskach K, Ferguson SH, Hare J, Stern G, Macinnis G, Marvin CH, Loseto L (2009) Trophodynamics of some PFCs and BFRs in a Western Canadian arctic marine food web. Environ Sci Technol 43:4076–4081

    Article  CAS  Google Scholar 

  31. Kelly BC, Ikonomou MG, Blair JD, Surridge B, Hoover D, Grace R, Gobas FAPC (2009) Perfluoroalkyl contaminants in an arctic marine food web: trophic magnification and wildlife exposure. Environ Sci Technol 43:4037–4043

    Article  CAS  Google Scholar 

  32. Reiner JL, O'Connell SG, Moors AJ, Kucklick JR, Becker PR, Keller JM (2011) Spatial and temporal trends of perfluorinated compounds in Beluga whales (Delphinapterus leucas) from Alaska. Environ Sci Technol 45:8129–8136

    Article  CAS  Google Scholar 

  33. Taniyasu S, Kannan K, So MK, Gulkowska A, Sinclair E, Okazawa T, Yamashita N (2005) Analysis of fluorotelomer alcohols, fluorotelomer acids, and short- and long-chain perfluorinated acids in water and biota. J Chromatogr A 1093:89–97

    Article  CAS  Google Scholar 

  34. Hansen KJ, Clemen LA, Ellefson ME, Johnson HO (2001) Compound-specific, quantitative characterization of organic fluorochemicals in biological matrices. Environ Sci Technol 35:766–770

    Article  CAS  Google Scholar 

  35. Muller CE, De Silva AO, Small J, Williamson M, Wang X, Morris A, Katz S, Gamberg M, Muir DC (2011) Biomagnification of perfluorinated compounds in a remote terrestrial food chain: Lichen-Caribou-Wolf. Environ Sci Technol 45:8665–8673

    Article  CAS  Google Scholar 

  36. De Silva AO, Spencer C, Scott BF, Backus S, Muir DCG (2011) Detection of a cyclic perfluorinated acid, perfluoroethylcyclohexane sulfonate, in the Great Lakes of North America. Environ Sci Technol 45:8060–8066

    Article  Google Scholar 

  37. Malinsky MD, Jacoby CB, Reagen WK (2011) Determination of perfluorinated compounds in fish fillet homogenates: method validation and application to fillet homogenates from the Mississippi River. Anal Chim Acta 683:248–257

    Article  CAS  Google Scholar 

  38. Powley CR, George SW, Ryan TW, Buck RC (2005) Matrix effect-free analytical methods for determination of perfluorinated carboxylic acids in environmental matrixes. Anal Chem 77:6353–6358

    Article  CAS  Google Scholar 

  39. Kwadijk CJAF, Korytar P, Koelmans AA (2010) Distribution of perfluorinated compounds in aquatic systems in The Netherlands. Environ Sci Technol 44:3746–3751

    Article  CAS  Google Scholar 

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Acknowledgement

We would like to thank S. Leigh of the NIST Statistical Engineering Division for statistical analysis of the results as part of the value-assignment process for the SRMs. We would also like to thank Mary Williamson, from the Water Science and Technology Directorate, Burlington, for her help in the analyses of SRMs 1946 and 1947.

Disclaimer

Specific commercial equipment, instruments, or materials are identified in this paper to specify adequately the experimental procedure. Such identification does not imply recommendation or endorsement by the National Institute of Standards and Technology, nor does it imply that the materials or equipment identified are necessarily the best available for the purpose.

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Correspondence to Jessica L. Reiner.

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Published in the topical collection Emerging Contaminants in Biota with guest editors Yolanda Picó and Damià Barceló.

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Reiner, J.L., O’Connell, S.G., Butt, C.M. et al. Determination of perfluorinated alkyl acid concentrations in biological standard reference materials. Anal Bioanal Chem 404, 2683–2692 (2012). https://doi.org/10.1007/s00216-012-5943-5

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  • DOI: https://doi.org/10.1007/s00216-012-5943-5

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