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Determination of microcystins in natural blooms and cyanobacterial strain cultures by matrix solid-phase dispersion and liquid chromatography–mass spectrometry

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Abstract

An analytical procedure based on matrix solid-phase dispersion (MSPD) and liquid chromatography–mass spectrometry (LC-MS) was developed for determining three microcystins (MCs) in natural water blooms and cyanobacteria strain cultures. The procedure involves sample homogenization with C18, washed with dichloromethane to eliminate interfering compounds, and elution with acidic methanol. Results were compared to those achieved by using an organic solvent standard method. Mean recoveries of MCs with MSPD were 85–92% with intra-day relative standard deviation (RSDs) of 9–19%, whereas organic solvent extraction resulted in recovery rates of 92–105% with intra-day RSDs ranging from 8 to 18%. Limits of quantification (LOQs) were 1 μg g−1 dry weight for the MCs either by MSPD or organic solvent extraction. The two analytical methods tested were specific and sensitive to the extraction of MCs and were applied to the detection of MCs in water blooms and culture strains. The concentration of MCs varied from 7 to 3,330 μg g−1 of lyophilized cells with MC-LR always showing the highest concentration. MCs levels were higher in culture strains than in water blooms, except for MC-LR, whose concentration in blooms was slightly superior to that determined in culture strains.

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Acknowledgements

The authors wish thank Dr. Susana Franca and Dr. Paulo Pereira (Instituto Nacional de Saude Dr. Ricardo Jorge, Lisboa, Portugal) for the supply of the lyophilized blooms of cyanobacteria and the CICYT (AGL 2002-02622) for the financial support of this project.

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Authors and Affiliations

  1. Laboratori de Bromatologia i Toxicologia, Facultad de Farmàcia, Universitat de València, 46100, Burjassot, Valencia, Spain

    María J. Ruiz & Yolanda Picó

  2. Área de Toxicología, Facultad de Farmacia, Universidad de Sevilla, C/ Profesor García González s/n, 41012, Sevilla, Spain

    Ana Cameán & Isabel M. Moreno

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  1. Ana Cameán
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  2. Isabel M. Moreno
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  3. María J. Ruiz
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  4. Yolanda Picó
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Correspondence to Yolanda Picó.

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Cameán, A., Moreno, I.M., Ruiz, M.J. et al. Determination of microcystins in natural blooms and cyanobacterial strain cultures by matrix solid-phase dispersion and liquid chromatography–mass spectrometry. Anal Bioanal Chem 380, 537–544 (2004). https://doi.org/10.1007/s00216-004-2755-2

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  • DOI: https://doi.org/10.1007/s00216-004-2755-2

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