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Liquid chromatography coupled with tandem mass spectrometry to characterise trace levels of cyanobacteria and dinoflagellate toxins in suspended solids and sediments

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Abstract

Microcystins, anatoxins and okadaic acid are toxins produced by freshwater cyanobacteria and marine dinoflagellates. These toxins have been the responsible for the illness and death of biota and humans. To determine their presence in water during blooms, sensitive analytical methods are needed. In this study, we have developed a new liquid chromatography tandem mass spectrometry (LC-MS/MS) method for fast multiresidue determination of five toxins in suspended material and sediment samples. For each target compound, two selected reaction monitoring (SRM) transitions were optimised. Chromatographic conditions were optimised considering that the compounds analysed had different chemical structure and chromatographic behaviour. Using a Luna C18 column and specific SRM transitions, five phytotoxins were resolved. Method detection limits (MDL) for anatoxin-a, microcystins RR, LR and YR and okadaic acid were 7.1, 3.3, 81.7, 102.8 and 28.8 ng g−1 dry weight in sediment, respectively. The developed analytical method was successfully applied to analyse the presence of toxins in suspended solids and sediment from Ebro River (NE Spain) and Ebro delta-associated lagoons. Anatoxin-a was detected downstream of the Riba-Roja reservoir with levels ranging from 20 to 1120 ng g−1 dry weight of suspended solids. Okadaic acid was only detected in three samples collected in the Alfacs Bay (Ebro delta, Spain) affected by Dinophysis blooms in 2012.

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Acknowledgements

This work was supported by the Spanish MICINN grant and FEDER funds (CTM2011-30471-C02-01). Claudia Rivetti was supported by a fellowship from the MICINN (FPI BES-2012-053631). We thank Jorge Diogène, head of the Marine Monitoring Subprogram of IRTA, Sant Carles de la Ràpita, 43540, Spain for kindly supplying the Dinophysis bloom samples.

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  1. Department of Environmental Chemistry, IDAEA-CSIC, Jordi Girona 18, 08034, Barcelona, Spain

    Claudia Rivetti, Cristian Gómez-Canela, Silvia Lacorte & Carlos Barata

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  1. Claudia Rivetti
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  2. Cristian Gómez-Canela
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  3. Silvia Lacorte
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  4. Carlos Barata
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Correspondence to Carlos Barata.

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Rivetti, C., Gómez-Canela, C., Lacorte, S. et al. Liquid chromatography coupled with tandem mass spectrometry to characterise trace levels of cyanobacteria and dinoflagellate toxins in suspended solids and sediments. Anal Bioanal Chem 407, 1451–1462 (2015). https://doi.org/10.1007/s00216-014-8308-4

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  • DOI: https://doi.org/10.1007/s00216-014-8308-4

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