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Screen-printed electrode-based electrochemical detector coupled with in-situ ionic-liquid-assisted dispersive liquid–liquid microextraction for determination of 2,4,6-trinitrotoluene

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Abstract

A novel method is reported, whereby screen-printed electrodes (SPELs) are combined with dispersive liquid–liquid microextraction. In-situ ionic liquid (IL) formation was used as an extractant phase in the microextraction technique and proved to be a simple, fast and inexpensive analytical method. This approach uses miniaturized systems both in sample preparation and in the detection stage, helping to develop environmentally friendly analytical methods and portable devices to enable rapid and onsite measurement. The microextraction method is based on a simple metathesis reaction, in which a water-immiscible IL (1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide, [Hmim][NTf2]) is formed from a water-miscible IL (1-hexyl-3-methylimidazolium chloride, [Hmim][Cl]) and an ion-exchange reagent (lithium bis[(trifluoromethyl)sulfonyl]imide, LiNTf2) in sample solutions. The explosive 2,4,6-trinitrotoluene (TNT) was used as a model analyte to develop the method. The electrochemical behavior of TNT in [Hmim][NTf2] has been studied in SPELs. The extraction method was first optimized by use of a two-step multivariate optimization strategy, using Plackett–Burman and central composite designs. The method was then evaluated under optimum conditions and a good level of linearity was obtained, with a correlation coefficient of 0.9990. Limits of detection and quantification were 7 μg L−1 and 9 μg L−1, respectively. The repeatability of the proposed method was evaluated at two different spiking levels (20 and 50 μg L−1), and coefficients of variation of 7 % and 5 % (n = 5) were obtained. Tap water and industrial wastewater were selected as real-world water samples to assess the applicability of the method.

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Acknowledgments

The authors would like to thank the Spanish Ministry of Science and Innovation (project n. CTQ2011-23968), Generalitat Valenciana (Spain) (projects n. ACOMP/2013/072 and PROMETEO/2012/038) and Universidad de Alicante (Spain) (project n. GRE12-45) for the financial support. E.F. also thanks Generalitat Valenciana for her fellowship.

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Authors and Affiliations

  1. Departamento de Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Universidad de Alicante, P.O. Box 99, 03080, Alicante, Spain

    Elena Fernández, Lorena Vidal & Antonio Canals

  2. Departamento de Química Física e Instituto Universitario de Electroquímica, Universidad de Alicante, P.O. Box 99, 03080, Alicante, Spain

    Jesús Iniesta

  3. Faculty of Science and Engineering, Chemistry and Environmental Science, Manchester Metropolitan University, Chester Street, Manchester, M1 5GD, UK

    Jonathan P. Metters & Craig E. Banks

Authors
  1. Elena Fernández
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  2. Lorena Vidal
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  3. Jesús Iniesta
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  4. Jonathan P. Metters
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  5. Craig E. Banks
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  6. Antonio Canals
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Corresponding authors

Correspondence to Lorena Vidal or Antonio Canals.

Additional information

Published in the topical collection Microextraction Techniques with guest editors Miguel Valcárcel Cases, Soledad Cárdenas Aranzana and Rafael Lucena Rodríguez.

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Fernández, E., Vidal, L., Iniesta, J. et al. Screen-printed electrode-based electrochemical detector coupled with in-situ ionic-liquid-assisted dispersive liquid–liquid microextraction for determination of 2,4,6-trinitrotoluene. Anal Bioanal Chem 406, 2197–2204 (2014). https://doi.org/10.1007/s00216-013-7415-y

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  • DOI: https://doi.org/10.1007/s00216-013-7415-y

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