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The determination of pharmaceutical residues in cooked and uncooked marine bivalves using pressurised liquid extraction, solid-phase extraction and liquid chromatography–tandem mass spectrometry

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Abstract

An optimised and validated method for the determination of pharmaceutical residues in blue mussels (Mytilus spp.) is presented herein, as well as an investigation of the effect of cooking (by steaming) on any potential difference in human exposure risk. Selected pharmaceuticals included two non-steroidal anti-inflammatory drugs (diclofenac and mefenamic acid), an antibiotic (trimethoprim), an anti-epileptic (carbamazepine) and a lipid regulator (gemfibrozil). An in vivo exposure experiment was set up in the laboratory in which mussels were exposed either directly by injection (10 ng) or daily through spiked artificial seawater (ASW) over 96 h. In liquid matrices, pharmaceutical residues were either determined using liquid chromatography–tandem mass spectrometry (LC-MS/MS) directly, or in combination with solid-phase extraction (SPE) for analyte concentration purposes. The extraction of pharmaceuticals from mussel tissues used an additional pressurised liquid extraction step prior to SPE and LC-MS/MS. Limits of quantification of between 2 and 46 ng L−1 were achieved for extracted cooking water and ASW, between 2 and 64 μg L−1 for ASW in exposure tanks, and between 4 and 29 ng g−1 for mussel tissue. Method linearities were achieved for pharmaceuticals in each matrix with correlation coefficients of R 2 > 0.975. A selection of exposed mussels was also cooked (via steaming) and analysed using the optimised method to observe any effect on detectable concentrations of parent pharmaceuticals present. An overall increase in pharmaceutical residues in the contaminated mussel tissue and cooking water was observed after cooking.

Pharmaceutical residues in cooked and uncooked marine bivalves

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Acknowledgments

The authors would like to thank Lynn Vanhaecke and Julie Kiebooms of Ghent University for their assistance with method development. This report is published as part of the Science, Technology, Research and Innovation for the Environment (STRIVE) Programme 2007–2013 which is funded by the Irish Government under the National Development Plan 2007–2013 and administered on behalf of the Department of the Environment, Heritage and Local Government by the Environmental Protection Agency. This research is also partly funded by Science Foundation of Ireland (Grant Number 08/SRC/B1412).

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Authors and Affiliations

  1. Irish Separation Science Cluster (ISSC), Dublin City University, Glasnevin, Dublin 9, Ireland

    Gillian McEneff & Brian Kelleher

  2. Irish Centre for Environmental Toxicology (ICET), Galway-Mayo Institute of Technology, Dublin Road, Galway, Ireland

    Gillian McEneff & Brian Quinn

  3. Analytical & Environmental Sciences Division, School of Biomedical Sciences, King’s College London, Franklin-Wilkins Building, 150 Stamford St., London, SE1 9NH, UK

    Leon Barron

  4. School of Chemical Sciences, Dublin City University, Glasnevin, Dublin 9, Ireland

    Brian Kelleher

  5. Australian Centre for Research on Separation Science (ACROSS), School of Chemistry, University of Tasmania, Private Bag 75, Hobart, TAS, 7001, Australia

    Brett Paull

  6. Institute of Biomedical and Environmental Health Research (IBEHR), University of the West of Scotland, Paisley, PA1 2BE, Scotland, UK

    Brian Quinn

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  1. Gillian McEneff
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  2. Leon Barron
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Correspondence to Gillian McEneff.

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McEneff, G., Barron, L., Kelleher, B. et al. The determination of pharmaceutical residues in cooked and uncooked marine bivalves using pressurised liquid extraction, solid-phase extraction and liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 405, 9509–9521 (2013). https://doi.org/10.1007/s00216-013-7371-6

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