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Membrane-assisted solvent extraction coupled to large volume injection–gas chromatography–mass spectrometry for the determination of a variety of endocrine disrupting compounds in environmental water samples

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Abstract

Membrane-assisted solvent extraction coupled to large volume injection in a programmable temperature vaporisation injector using gas chromatography–mass spectrometry analysis was optimised for the simultaneous determination of a variety of endocrine disrupting compounds in environmental water samples (estuarine, river and wastewater). Among the analytes studied, certain hormones, alkylphenols and bisphenol A were included. The nature of membranes, extraction solvent, extraction temperature, solvent volume, extraction time, ionic strength and methanol addition were evaluated during the optimisation of the extraction. Matrix effects during the extraction step were studied in different environmental water samples: estuarine water, river water and wastewater (influent and effluent). Strong matrix effects were observed for most of the compounds in influent and effluent samples. Different approaches were studied in order to correct or minimise matrix effects, which included the use of deuterated analogues, matrix-matched calibration, standard addition calibration, dilution of the sample and clean-up of the extract using solid-phase extraction (SPE). The use of deuterated analogues corrected satisfactorily matrix effect for estuarine and effluent samples for most of the compounds. However, in the case of influent samples, standard addition calibration and dilution of the sample were the best approaches. The SPE clean-up provided similar recoveries to those obtained after correction with the corresponding deuterated analogue but better chromatographic signal was obtained in the case of effluent samples. Method detection limits in the 5–54 ng L−1 range and precision, calculated as relative standard deviation, in the 2–25% range were obtained.

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Acknowledgements

This work was financially supported by the Spanish Ministry of Science and Innovation through the CTQ2008-02775/BQU project and the University of the Basque Country through the UNESCO07/09 project. A. Iparraguirre and A. Prieto are grateful to the Basque Government for their pre-doctoral and post-doctoral fellowships, respectively. R. Rodil extends her gratitude to the Spanish Ministry of Science and Innovation for her Ramón y Cajal research contract.

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Authors and Affiliations

  1. Department of Analytical Chemistry, University of the Basque Country (UPV/EHU), P.K. 644, 48080, Bilbao, Spain

    Arantza Iparraguirre, Patricia Navarro, Ailette Prieto, Maitane Olivares, Luis-Ángel Fernández & Olatz Zuloaga

  2. IKERBASQUE, Basque Foundation for Science, 48011, Bilbao, Spain

    Ailette Prieto

  3. Department of Analytical Chemistry, Helmholtz Centre for Environmental Research, UFZ Permoserstraße 15, 04318, Leipzig, Germany

    Ailette Prieto

  4. Department of Analytical Chemistry, University of Santiago de Compostela, Constantino Candeira s/n, 15782, Santiago de Compostela, Spain

    Rosario Rodil

Authors
  1. Arantza Iparraguirre
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  2. Patricia Navarro
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  3. Ailette Prieto
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  4. Rosario Rodil
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  5. Maitane Olivares
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  6. Luis-Ángel Fernández
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  7. Olatz Zuloaga
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Corresponding author

Correspondence to Patricia Navarro.

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Iparraguirre, A., Navarro, P., Prieto, A. et al. Membrane-assisted solvent extraction coupled to large volume injection–gas chromatography–mass spectrometry for the determination of a variety of endocrine disrupting compounds in environmental water samples. Anal Bioanal Chem 402, 2897–2907 (2012). https://doi.org/10.1007/s00216-012-5717-0

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  • DOI: https://doi.org/10.1007/s00216-012-5717-0

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