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Rapid clean-up and effective sample preparation procedure for unambiguous determination of the cyclic peptides microcystin and nodularin

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Summary

A new sample preparation strategy has been established to improve the identification and determination of nodularin and microcystins. The sample preparation consisted of enrichment of the analytes by solid phase extraction with C18 cartridges followed by clean-up of the enriched raw extracts by high performance size exclusion gel permeation chromatography. In contrast to established clean-up procedures based on polarity, related distribution of microcystins and nodularin in non-miscible phases (e. g. a C18 cartridge as stationary phase and a water-containing eluent as mobile phase) this strategy separates microcystins from interfering compounds by molecular size differences.

The sample preparation procedure can be automated easily and was validated for both water samples as well as raw extracts of algal cells. The method was success-fully applied during an experiment with natural algae communities from the Baltic Sea to investigate the influence of different nutrient limitations on toxicity ofNodularia sp...

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References

  1. W. W. Carmichael, inC. L. Ownby andG. V. Odell (Eds.), Natural Toxins. Characterization, Pharmacology and Therapeutics. Proceedings of the 9th World Congress on Animal, Plant and Microbial Toxis, Freshwater Cyanobacteria (bluegreen algae) Toxins, Stillwater, August 1988, Oklahoma, USA, Pergamon Press, New York, USA, 1988, p. 3

    Google Scholar 

  2. W. W. Carmichael, J. Appl. Bact.,72, 445 (1992)

    CAS  Google Scholar 

  3. W. W. Carmichael, spektrum der Wissenschaft70 (1994)

  4. G. A. Codd, Water Science and Technology32, 149 (1995)

    Article  CAS  Google Scholar 

  5. K. Sivonen, Phycologia35, 12 (1996)

    Article  Google Scholar 

  6. R. M. Dawson Toxicon36, 953 (1998)

    Article  CAS  Google Scholar 

  7. M. Namikoshi, K. L. Rinehart, R. Sakai, K. Sivonen, W. W. Carmichael. J. Org. Chem.55, 6135 (1990)

    Article  CAS  Google Scholar 

  8. K. Sivonen, W. W. Carmichael, M. Namikoshi, K. L. Rinehart, A. M. Dahlem, S. I. Niemela, Appl. Environ. Microbiol.56, 2650 (1990)

    CAS  Google Scholar 

  9. K. I. Harada, K. Ogawa, K. Matsuura, H. Nagai, H. Murata, M. Suzuki, P. M. Thorn, Y. Itezono, N. Nakayama, M. Shirai, M. Nakano, Toxicon29, 479 (1991)

    Article  CAS  Google Scholar 

  10. M. Namikoshi, K. Sivonen, W. R. Evans, W. W. Carmichael, L. Rouhiainen, R. Luukkainen, K. L. Rinehart, Toxicol.5, 661 (1992)

    CAS  Google Scholar 

  11. M. Namikoshi, K. Sivonen, W. R. Evans, W. W. Carmichael, L. Rouhiainen, R. Luukkainen, K. L. Rinehart. Toxicon30, 1457 (1992)

    Article  CAS  Google Scholar 

  12. K. Sivonen, M. Namikoshi, W. R. Evans, B. V. Gromov, W. W. Carmichael, K. L. Rinehart. Toxicon,30, 1481 (1992)

    Article  CAS  Google Scholar 

  13. K. Sivonen, M. Namikoshi, W. E. Evans, M. Fardig, W. W. Carmichael, K. L. Rinehart. Chem. Res. Toxicol.5, 464 (1992)

    Article  CAS  Google Scholar 

  14. M. Namikoshi, K. L. Rinehart, R. Sakai, R. R. Stotts, A. M. Dahlem, V. R. Beasley, W. W. Carmichael, W. R. Evans. J. Org. Chem.57, 866 (1992)

    Article  CAS  Google Scholar 

  15. R. Luukkainen, M. Namikoshi, K. Sivonen, K. L. Rinehart, S. I. Niemelä. Toxicon32, 133 (1994)

    Article  CAS  Google Scholar 

  16. R. E. Honkanen, B. A. Codispoti, K. Tse, A. L. Boynton, Toxicon32, 339 (1994)

    Article  CAS  Google Scholar 

  17. M. Namikoshi, M. Yuan, K. Sivonen, W. W. Carmichael, K. L. Rinehart, L. Rouhiainen, F. Sun, S. Brittain, A. Otsuki, Chem Res Toxicol.11 (2), 143 (1998)

    Article  CAS  Google Scholar 

  18. E. M. Jochimsen, W. W. Carmichael, J. An, D. M. Cardo, S. T. Cookson, C. E. M. Holmes, M. B. C. Antunes, D. A. Melo Filho, T. M. Lyra, V. S. T. Baretto, S. M. F. O. Azevedo, W. R. Jarvis. N Engl J Med.338 (13), 873 (1998)

    Article  CAS  Google Scholar 

  19. M. T. Runnegar, J. R. Falconer, Toxicon24, 109 (1986)

    Article  CAS  Google Scholar 

  20. K. -I. Harada, K. Matsuura, M. Suzuki, J. Chromatogr.448, 275 (1988)

    Article  CAS  Google Scholar 

  21. G. A. Codd, S. G. Bell, W. P. Brooks, Water Sci. Technol.21, 1 (1989)

    CAS  Google Scholar 

  22. R. Matsushima, S. Yoshizawa, M. E. Watanabe, K. I. Harada, M. Furusawa, W. W. Carmichael, Biochem. Biophys. Res. Commun.171, 867 (1990)

    Article  CAS  Google Scholar 

  23. S. G. Bell, G. A. Codd, Reb. Med. Microbiol.,5, 256 (1994)

    Google Scholar 

  24. I. R. Falconer, T. H. Buckley, Med. J. Aust.150, 351 (1989)

    CAS  Google Scholar 

  25. R. Nishiwaki-Matsushima, T. Ohta, S. Nishiwaki, M. Suganuma, K. Kohyama, T. Ishikawa, W. W. Carmichael, H. Fujiki, J. Cancer Res. Clin. Oncol.118, 420 (1992)

    Article  CAS  Google Scholar 

  26. I. R. Falconer, Phycologia35 (Suppl), 6 (1996)

    Article  Google Scholar 

  27. L. Lawton, C. Edwards, G. A. Codd, Analyst,119, 1525 (1994)

    Article  CAS  Google Scholar 

  28. K. I. Harada, Phycologia35 (Suppl), 36 (1996)

    Article  Google Scholar 

  29. K. Harada, M. Oshikata, T. Shimada, A. Nagata, N. Ishikawa, M. Suzuki, F. Kondo, M. Shimizu, S. Yamadá, Nat Toxins5 (5), 201 1997

    Article  CAS  Google Scholar 

  30. J. An, W. W. Carmichael, Toxicon32, 1495 (1994)

    Article  CAS  Google Scholar 

  31. R. E. Honkanen, B. A. Codispoti, K. Tse, Toxicon32, 339 (1994)

    Article  CAS  Google Scholar 

  32. W. W. Carmichae, P. E. Bent, Applied and Environmental Microbiology41 (6), 1383 (1981)

    Google Scholar 

  33. E. Graneli, P. Carlsson, C. Legrand, G. Johnsen, S. Y. Maestrini, M. Reichelt (ASLO, Aquatic Sciences meeting, 1–5 February 1999, Santa Fe, USA), Structuration of marine phytoplankton communities subjected to different levels of N, P, and Si limitation in a mesocosm experiment. (abstract), in press.

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Authors and Affiliations

  1. Institute of Nutrition and Environment, University of Jena, Dornburger Str. 25a, 07743, Jena, Germany

    C. Hummert, M. Reichelt & B. Luckas

  2. Institute of Natural Sciences, University of Kalmar, Box 905, 39129, Kalmar, Sweden

    C. Legrand & E. Graneli

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  1. C. Hummert
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  2. M. Reichelt
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  3. C. Legrand
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  4. E. Graneli
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  5. B. Luckas
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Hummert, C., Reichelt, M., Legrand, C. et al. Rapid clean-up and effective sample preparation procedure for unambiguous determination of the cyclic peptides microcystin and nodularin. Chromatographia 50, 173–180 (1999). https://doi.org/10.1007/BF02490648

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  • DOI: https://doi.org/10.1007/BF02490648

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