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Determination of endocrine-disrupting compounds in water samples by magnetic nanoparticle-assisted dispersive liquid–liquid microextraction combined with gas chromatography–tandem mass spectrometry

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Abstract

A rapid extraction procedure is presented for the determination of five endocrine-disrupting compounds, estrone, ethinylestradiol, bisphenol A, triclosan, and 2-ethylhexylsalicylate, in water samples. The analysis involves a two-step extraction procedure that combines dispersive liquid–liquid microextraction (DLLME) with dispersive micro-solid phase extraction (D-μ-SPE), using magnetic nanoparticles, followed by in situ derivatization in the injection port of a gas chromatograph coupled to triple quadrupole mass spectrometry. The use of uncoated or oleate-coated Fe3O4 nanoparticles as sorbent in the extraction process was evaluated and compared. The main parameters involved in the extraction process were optimized applying experimental designs. Uncoated Fe3O4 nanoparticles were selected in order to simplify and make more cost-effective the procedure. DLLME was carried out at pH 3, during 2 min, followed by the addition of the nanoparticles for D-μ-SPE employing 1 min in the extraction. Analysis of spiked water samples of different sources gave satisfactory recovery results for all the compounds with detection limits ranging from 7 to 180 ng l−1. Finally, the procedure was applied in tap, well, and river water.

Diagram of the extraction method using magnetic nanoparticles (MNPs)

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Acknowledgments

This study was financed by the Ministry of Science and Innovation–National Institute for Agricultural and Food Research and Technology, INIA, Project number RTA2014-00012-C03-01. The authors wish to express their gratefulness to Dr. M.P. Morales, researcher of the Department of Biomaterials and Bioinspired Materials (ICMM; CSIC), for her help and advice in the characterization of the MNPs and to the microanalysis laboratory of the Institute of General Organic Chemistry (CSIC) for the elemental analysis of the MNPs.

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Authors and Affiliations

  1. Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Carretera de la Coruña 7, 28040, Madrid, Spain

    Rosa Ana Pérez, Beatriz Albero, José Luis Tadeo & Consuelo Sánchez-Brunete

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  1. Rosa Ana Pérez
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  2. Beatriz Albero
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  4. Consuelo Sánchez-Brunete
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Correspondence to Rosa Ana Pérez.

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Pérez, R.A., Albero, B., Tadeo, J.L. et al. Determination of endocrine-disrupting compounds in water samples by magnetic nanoparticle-assisted dispersive liquid–liquid microextraction combined with gas chromatography–tandem mass spectrometry. Anal Bioanal Chem 408, 8013–8023 (2016). https://doi.org/10.1007/s00216-016-9899-8

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  • DOI: https://doi.org/10.1007/s00216-016-9899-8

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