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Results of a European interlaboratory method validation study for the quantitative determination of lipophilic marine biotoxins in raw and cooked shellfish based on high-performance liquid chromatography–tandem mass spectrometry. Part I: collaborative study

Abstract

A European interlaboratory collaborative study was conducted to validate a method for the quantitative determination of lipophilic marine biotoxins based on high-performance liquid chromatography–tandem mass spectrometry. During this study, the diarrhetic shellfish poisoning toxins okadaic acid, dinophysis toxin1 and 2 including their esters, the azaspiracids 1-3, pectenotoxin2, and the yessotoxins were investigated at concentration levels near the limit of quantification and near the legal limit. Naturally contaminated blue mussels, both raw and cooked and spiked extracts of clams and oysters were studied and results were obtained for 16 test samples from 16 laboratories representing eight different countries. This article summarizes the study outcome concerning validation key parameters like specificity, linearity, limit of detection, accuracy/recovery, and precision. Further, influences of cooking of mussels before homogenization or hydrolysis on method robustness have been evaluated.

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References

  1. European Union (2004) Brussels. Off J Eur Union L 226:22

    Google Scholar 

  2. EFSA (2008) EFSA J 589:1–62

    Google Scholar 

  3. EFSA (2008) EFSA J 723:1–52

    Google Scholar 

  4. EFSA (2008) EFSA J 907:1–62

    Google Scholar 

  5. EFSA (2009) EFSA J 1109:1–47

    Google Scholar 

  6. European Union (2005) Brussels. Off J Eur Union L 338:27

    Google Scholar 

  7. McNabb P, Selwood AI, Holland PT (2005) J AOAC Int 88:761–772

    CAS  Google Scholar 

  8. European Union. (EC) No 854/2004

  9. Horwitz W (1995) Pure Appl Chem 67:331–343

    Article  Google Scholar 

  10. Mountfort DO, Suzuki T, Truman P (2000) Toxicon 39:383–390

    Article  Google Scholar 

  11. Thompson M, Wood R (1993) J AOAC Int 76:926–940

    Google Scholar 

  12. Horwitz W, Kamps LR, Boyer KW (1980) J Assoc Off Anal Chem 63:1344–1354

    CAS  Google Scholar 

  13. ISO 11843: Capability of detection, June 2006. 2010

  14. ISO 5725-3. (including Technical Corrigendum). 2001

  15. Thompson M (2000) Analyst 125:385–386

    Article  CAS  Google Scholar 

  16. Careri M, Mangia A (2006) Anal Bioanal Chem 386:38–45

    Article  CAS  Google Scholar 

  17. Fux E, Rode D, Bire R, Hess P (2008) Food Addit Contam 25:1024–1032

    Article  CAS  Google Scholar 

  18. Gerssen A, McElhinney MA, Mulder PPJ, Bire R, Hess P, de Boer J (2009) Anal Bioanal Chem 394:1213–1226

    Article  CAS  Google Scholar 

  19. These A, Scholz J, Preiss-Weigert A (2009) J Chromatogr A 1216:4529–4538

    Article  CAS  Google Scholar 

  20. Hess P, Nguyen L, Aasen J, Keogh M, Kilcoyne J, McCarron P, Aune T (2005) Toxicon 46:62–71

    Article  CAS  Google Scholar 

  21. Rodrigues SM, Vale P, Botelho MJ, and Gomes SS (2009) Food Additives and Contaminants Part A—Chemistry Analysis Control Exposure & Risk Assessment 26:229-235

    Google Scholar 

  22. Lee JS, Yanagi T, Kenma R, Yasumoto T (1987) Agric Biol Chem 51:877–881

    Article  CAS  Google Scholar 

  23. Gerssen A, van Olst EHW, Mulder PPJ, de Boer J (2010) Anal Bioanal Chem 397:3079–3088

    Article  CAS  Google Scholar 

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Acknowledgment

We thank Margarete Schramm for her careful organization of the laboratory work, especially the skilful preparation of samples and calibrants. Furthermore, we thank the competent agencies, the National Reference Laboratories of Norway and Ireland, for having kindly provided contaminated samples for analytical purposes.

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Correspondence to Anja These.

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Collaborators: Z. Amzil, M. Baden, C. Duffy, S. Effkemann, F. Gassmann, L. Heinze, P. Hess, G. Hochreuther, W. Hoebel, A. Johansson, K. Jorgensen, R. Kelly, O. Keuth, I. Lange, B. Luckas, A. Milandri, A. Miller, S. Morris, A.Z. Muratovic, I. Nausch, S. O´Brian, S. Pigozzi, P. Resch, K. Soellner, M.L. Rodriguez Velasco, M. Schramm, U. Schwank, M. Sibat, G. Thielert, C. Wiedow

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These, A., Klemm, C., Nausch, I. et al. Results of a European interlaboratory method validation study for the quantitative determination of lipophilic marine biotoxins in raw and cooked shellfish based on high-performance liquid chromatography–tandem mass spectrometry. Part I: collaborative study. Anal Bioanal Chem 399, 1245–1256 (2011). https://doi.org/10.1007/s00216-010-4383-3

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  • DOI: https://doi.org/10.1007/s00216-010-4383-3

Keywords

  • Lipophilic marine biotoxins
  • Okadaic acid
  • Azaspiracid
  • Pectenotoxin
  • Yessotoxin
  • Mass spectrometry
  • Collaborative study
  • Validation study