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Microwave-assisted extraction followed by headspace solid-phase microextraction and gas chromatography with mass spectrometry detection (MAE-HSSPME-GC-MS/MS) for determination of polybrominated compounds in aquaculture samples

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Abstract

This paper describes the first validated method for the extraction, purification and determination of trace levels of a number of pollutants of growing concern, including polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs), in aquaculture feeds and products. The new procedure comprises microwave-assisted extraction (MAE; optimized, using a central composite experimental design, to 15 min at 85 °C in 14 mL of 1:1 hexane/dichloromethane), and concentration by headspace solid-phase microextraction (HSSPME), and separation/quantification by gas chromatography with mass spectrometry detection (GC-MS/MS). The method was validated on the reference materials IAEA-406 and WMF-01. Limits of detection for fourteen of the fifteen analytes considered range from 10 to 600 pg g−1, and limits of quantification from 50 pg g−1 to 1.9 ng g−1. Linear ranges, accuracies and precisions are reported.

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Acknowledgements

This research was supported by the Project BQU2003-02090 (Spanish Commission for Research and Development MCYT-DGI). The authors kindly thank the Translation Service of the USC.

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Authors and Affiliations

  1. Instituto de Investigación y Análisis Alimentario (IIAA), Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Química, Universidad de Santiago de Compostela, Avda. de las Ciencias s/n, 15782, Santiago de Compostela, Spain

    A. M. Carro, R. A. Lorenzo, F. Fernández, R. Phan-Tan-Luu & R. Cela

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  1. A. M. Carro
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  2. R. A. Lorenzo
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  3. F. Fernández
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  4. R. Phan-Tan-Luu
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  5. R. Cela
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Correspondence to A. M. Carro.

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Carro, A.M., Lorenzo, R.A., Fernández, F. et al. Microwave-assisted extraction followed by headspace solid-phase microextraction and gas chromatography with mass spectrometry detection (MAE-HSSPME-GC-MS/MS) for determination of polybrominated compounds in aquaculture samples. Anal Bioanal Chem 388, 1021–1029 (2007). https://doi.org/10.1007/s00216-007-1220-4

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  • DOI: https://doi.org/10.1007/s00216-007-1220-4

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