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Abstract
HPLC is a well established method for the congener selective analysis of microcystins (potent cyanobacterial hepatotoxins) in water samples or cyanobacterial cells. Its application to microcystin determination in sediments from aquatic ecosystems is still an emerging technique, often hampered by the inherent complexity of the matrix “sediment” that may lead to selectivity (and hence confidence) issues due to coeluting substances.
Using size exclusion chromatography cleanup, we could demonstrate that the confidence of microcystin analysis in sediments by HPLC with UV detection can be enhanced, yet the improvements are not always sufficient to yield unambiguous results. This drawback was avoided by employing mass spectrometric detection hyphenated to HPLC. The developed analysis protocol was applied to organic rich, silty sediments from Lake Federsee, a eutrophic lake in Southwestern Germany. Results from these experiments are presented, along with a discussion of artefacts arising from the esterification of the microcystins with methanol during sample handling.
ACKNOWLEDGMENTS
Financial support was provided by the State Institute for Environment, Measurement and Nature Conservation Baden-Württemberg (Project-Nr.: 4500004431). C.S. also acknowledges funding from a Landesgraduiertenförderung scholarship (state of Baden-Württemberg). We further thank Dr. Martin Wessels and coworkers (Institute for Lake Research, Langenargen) and Dr. Heinz Buchert (Institute of Analytical and Environmental Chemistry, Ulm University) for their helpful support during sampling, sample preparation, and sedimentology. We would finally like to thank Prof. Dr. Rolf Jürgen Behm and Dr. Rune Halseid (Institute of Surface Chemistry and Catalysis, Ulm University) for cooperation in LC/MS work.
Manuscript 6378