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Determination of chlorobenzenes in water samples based on fully automated microextraction by packed sorbent coupled with programmed temperature vaporization–gas chromatography–mass spectrometry

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Abstract

A fully automated method consisting of microextraction by packed sorbent (MEPS) coupled directly to programmed temperature vaporizer–gas chromatography–mass spectrometry (PTV–GC–MS) has been developed to determine the 12 chlorobenzene congeners (chlorobenzene; 1,2-, 1,3-, and 1,4-dichlorobenzene; 1,2,3-, 1,2,4-, and 1,3,5-trichlorobenzene; 1,2,3,4-, 1,2,3,5-, and 1,2,4,5-tetrachlorobenzene; pentachlorobenzene; and hexachlorobenzene) in water samples. The effects of the variables on MEPS extraction, using a C18 sorbent, and the instrumental PTV conditions were studied. The internal standard 1,4-dichlorobenzene d4 was used as a surrogate. The proposed method afforded good reproducibility, with relative standard deviations (RSD %) lower than 12 %. The limits of detection varied between 0.0003 μg L−1 for 1,2,3,4-tetrachlorobenzene and 0.07 μg L−1 for 1,3- and 1,4-dichlorobenzene, while those of quantification varied between 0.001 μg L−1 and 0.2 μg L−1 for the same compounds. Accuracy of the proposed method was confirmed by applying it to the determination of chlorobenzenes in different spiked water samples, including river, reservoir, and effluent wastewater.

Experimental setup for automated MEPS methodology

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Acknowledgments

The authors acknowledge the financial support of the DGI (CTQ2010-17514/BQU) and the Consejería de Educación y Cultura of the Junta de Castilla y León (GR87) for this research. G. Grueiro Noche acknowledges financial support from the Xunta de Galicia for the concession of a grant for “Consolidation and structuring of competitive research groups in the University System of Galicia, 2010-12” and Project 09MDS038103PR. The authors are grateful to Aqualia for providing the effluent wastewater samples from their Salamanca (Spain) wastewater treatment plant.

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Authors and Affiliations

  1. Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008, Salamanca, Spain

    María Esther Fernández Laespada, José Luis Pérez Pavón & Bernardo Moreno Cordero

  2. Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus da Zapateira s/n, 15071 A, Coruña, Spain

    Gloria Grueiro Noche & Soledad Muniategui Lorenzo

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  1. Gloria Grueiro Noche
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  2. María Esther Fernández Laespada
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  3. José Luis Pérez Pavón
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  4. Bernardo Moreno Cordero
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  5. Soledad Muniategui Lorenzo
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Correspondence to María Esther Fernández Laespada.

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Grueiro Noche, G., Fernández Laespada, M.E., Pérez Pavón, J.L. et al. Determination of chlorobenzenes in water samples based on fully automated microextraction by packed sorbent coupled with programmed temperature vaporization–gas chromatography–mass spectrometry. Anal Bioanal Chem 405, 6739–6748 (2013). https://doi.org/10.1007/s00216-013-7112-x

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  • DOI: https://doi.org/10.1007/s00216-013-7112-x

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