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Simultaneous determination of hexabromocyclododecane, tetrabromobisphenol A, and related compounds in sewage sludge and sediment samples from Ebro River basin (Spain)

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Abstract

This paper describes the development of a methodology for the simultaneous determination and quantification of hexabromocyclododecane (HBCD), tetrabromobisphenol A (TBBPA), and related compounds (bisphenol A, monobromobisphenol A, dibromobisphenol A, and tribromobisphenol A) in sludge and sediment samples. The selected method is based on an extraction with dichloromethane: methanol followed by purification via SPE C18 cartridges. Instrumental determination was carried out by liquid chromatography–quadrupole linear ion trap mass spectrometry (LC-QqLIT-MS), with quantification based on isotopic dilution method. Analyte recoveries were in the range of 39–120% and 88–126% for spiked sewage and sediment, respectively. Repeatability of replicate extractions was better than 13% relative standard deviation. Linearity was checked in the range of 0.05 and 25 injected nanograms. Limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.6 and 2.7 ng/g and 1.4 and 66 ng/g for sediment and sludge samples, respectively. The developed method was applied to sewage sludge and sediment samples collected along the Ebro River and Cinca River, one of its tributaries (northeast of Spain). TBBPA levels in sewage sludge ranged from not quantified to 1,329 ng/g dw, whereas levels in sediment samples were lower, between not detected and 15 ng/g dw. As regards HBCD, concentrations were between not detected and 375 ng/g for sludge samples and 0.8 and 1850 ng/g for sediments.

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Acknowledgements

This work was funded by the Spanish Ministry of Environment and Rural and Marine Media (Project MMAMRM-010/PC08/3-04) and by the Spanish Ministry of Science and Innovation through the projects CEMAGUA (CGL2007-64551/HID) and SOSTAQUA (led by Aguas de Barcelona and funded by CDTI within the framework of the Ingenio 2010 Programme under the CENIT call) and Consolider-Ingenio 2010 (CSD2009-00065). Paula Guerra acknowledges her grant from Department d’Innovació, Universitats i Empresa (2008FI_B 00755). We thank Dr. Göran Marsh (Department of Environmental Chemistry, Stockholm University, Sweden) for MonoBBPA, DiBBPA, and TriBBPA standards. Waters Corporation (USA) and Isolute (Sweden) are gratefully acknowledged for providing the solid-phase extraction cartridges. Technical assistance provided by D. Fanjul, R. Chaler, and M. Comesaña (IDAEA-CSIC) is also gratefully acknowledged.

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Authors and Affiliations

  1. Department of Environmental Chemistry, IDAEA-CSIC, Jordi Girona 18-26, 08034, Barcelona, Spain

    Paula Guerra, Ethel Eljarrat & Damià Barceló

  2. Catalan Institute for Water Research (ICRA), Parc Científic i Tecnològic de la Universitat de Girona, Pic de Peguera 15, 17003, Girona, Spain

    Damià Barceló

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  1. Paula Guerra
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  2. Ethel Eljarrat
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  3. Damià Barceló
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Correspondence to Ethel Eljarrat.

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Guerra, P., Eljarrat, E. & Barceló, D. Simultaneous determination of hexabromocyclododecane, tetrabromobisphenol A, and related compounds in sewage sludge and sediment samples from Ebro River basin (Spain). Anal Bioanal Chem 397, 2817–2824 (2010). https://doi.org/10.1007/s00216-010-3670-3

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  • DOI: https://doi.org/10.1007/s00216-010-3670-3

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