Analytical and Bioanalytical Chemistry

, Volume 399, Issue 3, pp 1245–1256 | Cite as

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

  • Anja TheseEmail author
  • Christine Klemm
  • Ingo Nausch
  • Steffen Uhlig
Original Paper


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.


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



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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Copyright information

© Springer-Verlag 2010

Authors and Affiliations

  • Anja These
    • 1
    Email author
  • Christine Klemm
    • 2
  • Ingo Nausch
    • 3
  • Steffen Uhlig
    • 4
  1. 1.Federal Institute for Risk Assessment—National Reference Laboratory for Marine Biotoxins GermanyBerlinGermany
  2. 2.Federal Office of Consumer Protection and Food SafetyBerlinGermany
  3. 3.Landeslabor Schleswig-HolsteinNeumuensterGermany
  4. 4.quo data GmbHDresdenGermany

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