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Optimisation of a selective method for the determination of organophosphorous triesters in outdoor particulate samples by pressurised liquid extraction and large-volume injection gas chromatography–positive chemical ionisation–tandem mass spectrometry

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Abstract

A selective analytical method for the determination of nine organophosphate triesters and triphenylphosphine oxide (TPPO) in outdoor particulate matter is presented. It involves a fully automated pressurised liquid extraction (PLE) step, integrating an alumina clean-up process, and subsequent determination by large-volume injection gas chromatography–positive chemical ionisation–tandem mass spectrometry (LVI-GC–PCI–MS/MS). The extraction variables (solvent, amount of adsorbent, temperature, time and number of cycles) were optimised using a multicriteria strategy which implements a desirability function that maximises both extraction and clean-up efficiencies while searching for the best-compromise PLE conditions. The final method affords quantification limits of between 0.01 and 0.3 μg g−1 and recoveries of >80%, with the exceptions of the most polar analytes, TCEP and TPPO (~65%) for both urban dust and PM10 samples. Moreover, the method permitted the levels of these compounds in dust deposited outdoors (between LOD and 0.5 μg g−1 for TEHP) and PM10 samples (between LOD and 2.4 μg m−3 for TiBP) to be measured and reported for the first time.

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Acknowledgements

J.B.Q. and R.R. acknowledge Xunta de Galicia and Ministerio de Educación y Ciencia for their contract sponsorship through the Isidro Parga Pondal and Juan de la Cierva research programs, respectively. This work was financially supported by Ministerio de Educación y Ciencia (project no. REN2003-08603-C04-01) and Xunta de Galicia (“Programa de consolidación e estruturación de unidades de investigación competitivas, en réxime de concorrencia competitiva 2006”).

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Authors and Affiliations

  1. IUMA—University Institute of Environment, University of A Coruña, Pazo da Lóngora, Liáns, 15179, Oleiros (A Coruña), Spain

    José Benito Quintana, Purificación López-Mahía & Darío Prada-Rodríguez

  2. Department of Analytical Chemistry, Faculty of Sciences, University of A Coruña, Campus A Zapateira S.N., 15071, A Coruña, Spain

    Rosario Rodil, Purificación López-Mahía, Soledad Muniategui-Lorenzo & Darío Prada-Rodríguez

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  1. José Benito Quintana
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  2. Rosario Rodil
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  3. Purificación López-Mahía
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  4. Soledad Muniategui-Lorenzo
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  5. Darío Prada-Rodríguez
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Correspondence to José Benito Quintana.

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Quintana, J.B., Rodil, R., López-Mahía, P. et al. Optimisation of a selective method for the determination of organophosphorous triesters in outdoor particulate samples by pressurised liquid extraction and large-volume injection gas chromatography–positive chemical ionisation–tandem mass spectrometry. Anal Bioanal Chem 388, 1283–1293 (2007). https://doi.org/10.1007/s00216-007-1338-4

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  • DOI: https://doi.org/10.1007/s00216-007-1338-4

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