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Domoic acid at trace levels in lagoon waters: assessment of a method using internal standard quantification

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Abstract

Domoic acid (DA) is a neurotoxin produced by different algae, including pennate diatoms, principally from the genus Pseudo-nitzschia, and it is the main cause of amnesic shellfish poisoning. Determination of this toxin in seawater samples is fundamental to define the real contamination risks for aquatic species. We have developed two very sensitive instrumental methods using hydrophilic interaction liquid chromatography coupled using tandem mass spectrometry in positive and negative polarity modes. Instrumental detection limits were 9 pg mL−1 for positive and 19 pg mL−1 for negative ionisation. A procedural method based on solid-phase extraction for the determination of dissolved DA present in seawater has been developed, and an extraction procedure was employed for the determination of the toxin in the particulate fraction. DA quantification was performed using the internal standard method to account for signals fluctuations and random errors during sample treatment. To our knowledge, this is the first study to use this quantification method for DA determination. Trueness, extraction yield, matrix effects, repeatability and procedural detection limits were evaluated during method validation. Procedural detection limits of 0.3 pg mL−1 (positive mode) and 0.6 pg mL−1 (negative mode) were found for the dissolved fraction, and absolute limits of 0.4 pg (positive mode) and 6.0 pg (negative mode) for particulate samples were obtained. The most sensitive method in positive mode was applied to define DA occurrence in the Venice Lagoon. Trace concentrations of domoic acid ranging from 1.5 to 16.2 pg mL−1 were found for the first time in the Venetian environment.

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Acknowledgements

This work was supported by the National Research Council of Italy (CNR). The authors gratefully acknowledge the help of ELGA LabWater in providing the PURELAB Option-R and Ultra Analytic systems, which produced the ultra-pure water used in these experiments.

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Authors and Affiliations

  1. Department of Environmental Sciences, Informatics and Statistics, University of Venice, Ca’ Foscari, Calle Larga Santa Marta 2137, 30123, Venice, Italy

    E. Barbaro, R. Piazza, C. Barbante & A. Gambaro

  2. Institute for the Dynamics of Environmental Processes, National Research Council of Italy, Dorsoduro 2137, 30123, Venice, Italy

    E. Barbaro, R. Zangrando, S. Rossi, W. R. L. Cairns, R. Piazza, F. Corami, C. Barbante & A. Gambaro

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  1. E. Barbaro
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Correspondence to E. Barbaro.

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ESM 1

Sampling details and description of the environmental parameters during analysis are provided. Figures include the sampling stations and the spatial distribution of DA (picograms per milliliter), P-PO4 3− (micromolars), Si-Si(OH)4 (micromolars), total inorganic nitrogen (TIN = N-NO3 - + N-NO2 - + N-NH4 +) (micromolars), chlorophyll a (micrograms per milliliter) and the ratio between chlorophyll a and pheophytin a (PDF 1682 kb)

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Barbaro, E., Zangrando, R., Rossi, S. et al. Domoic acid at trace levels in lagoon waters: assessment of a method using internal standard quantification. Anal Bioanal Chem 405, 9113–9123 (2013). https://doi.org/10.1007/s00216-013-7348-5

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  • DOI: https://doi.org/10.1007/s00216-013-7348-5

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