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Single drop microextraction and gas chromatography–mass spectrometry for the determination of diflufenican, mepanipyrim, fipronil, and pretilachlor in water samples

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Abstract

An analytical method for the determination of diflufenican, mepanipyrim, pretilachlor, and fipronil in water samples was developed using single drop microextraction in the direct immersion mode and gas chromatography–mass spectrometry. A factorial fractionated design of type 26–1 at two levels was performed, to study the influence of experimental variables such as ionic strength, pH, agitation speed, extraction time, drop volume, and sample volume. To establish the optimal conditions for the variables that were significant, a Doehlert design was performed. The optimum conditions of extraction were 1 μL of heptane immersed in 4.0 mL of sample with continuous agitation at 500 rpm for 30 min at room temperature. The developed method proved to have good linearity for the range studied. The detection limits were 0.07 μg L−1 for diflufenican, 0.03 μg L−1 for mepanipyrim, 0.08 μg L−1 for pretilachlor, and 1.39 μg L−1 for fipronil. The method was validated on river water samples, showing the absence of matrix effect and recoveries ranged from 90.1 to 107.8 %. The results show that the method developed is accurate, sensitive, rapid, simple, and low cost, so it is recommended for application in the analysis of these different classes of pesticides in water samples.

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Acknowledgments

The authors wish to thank CONDES-LUZ for providing financial support to carry out this research.

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Authors and Affiliations

  1. Laboratory of Analytical Chemistry and Electrochemistry, Faculty of Engineering, University of Zulia, P.O. Box 4011-A-526, Maracaibo, Venezuela

    Lilia Araujo, María E. Troconis, Dalia Cubillán, Jair Mercado, Noreiva Villa & Avismelsi Prieto

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  1. Lilia Araujo
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  2. María E. Troconis
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  3. Dalia Cubillán
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  4. Jair Mercado
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  5. Noreiva Villa
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  6. Avismelsi Prieto
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Correspondence to Lilia Araujo.

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Araujo, L., Troconis, M.E., Cubillán, D. et al. Single drop microextraction and gas chromatography–mass spectrometry for the determination of diflufenican, mepanipyrim, fipronil, and pretilachlor in water samples. Environ Monit Assess 185, 10225–10233 (2013). https://doi.org/10.1007/s10661-013-3327-8

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  • DOI: https://doi.org/10.1007/s10661-013-3327-8

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