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The development and optimization of a modified single-drop microextraction method for organochlorine pesticides determination by gas chromatography-tandem mass spectrometry

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Abstract

We have developed a new method for single-drop microextraction (SDME) for the preconcentration of organochlorine pesticides (OCP) from complex matrices. It is based on the use of a silicone ring at the tip of the syringe. A 5 μL drop of n-hexane is applied to an aqueous extract containing the OCP and found to be adequate to preconcentrate the OCPs prior to analysis by GC in combination with tandem mass spectrometry. Fourteen OCP were determined using this technique in combination with programmable temperature vaporization. It is shown to have many advantages over traditional split/splitless injection. The effects of kind of organic solvent, exposure time, agitation and organic drop volume were optimized. Relative recoveries range from 59 to 117 %, with repeatabilities of <15 % (coefficient of variation) were achieved. The limits of detection range from 0.002 to 0.150 μg kg−1. The method was applied to the preconcentration of OCPs in fresh strawberry, strawberry jam, and soil.

A representative figure for OCP analysis by a modified SDME method.

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Acknowledgments

This research was supported by a Ph.D.grant from FCT (Fundação para a Ciência e a Tecnologia- BD/47200/2008) and grant no. PEst-C/EQB/LA0006/2011.

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Authors and Affiliations

  1. REQUIMTE, Instituto Superior de Engenharia, Instituto Politécnico do Porto, Rua Drº António Bernardino de Almeida, 431, 4200-072, Porto, Portugal

    Virgínia C. Fernandes, Viswanathan Subramanian, Valentina F. Domingues & Cristina Delerue-Matos

  2. CIQ – Faculdade de Ciências da Universidade do Porto - Departamento de Química e Bioquímica, Rua do Campo Alegre, 687, 4169-007, Porto, Portugal

    Virgínia C. Fernandes & Nuno Mateus

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  1. Virgínia C. Fernandes
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  2. Viswanathan Subramanian
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  3. Nuno Mateus
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  4. Valentina F. Domingues
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  5. Cristina Delerue-Matos
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Correspondence to Valentina F. Domingues.

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Fernandes, V.C., Subramanian, V., Mateus, N. et al. The development and optimization of a modified single-drop microextraction method for organochlorine pesticides determination by gas chromatography-tandem mass spectrometry. Microchim Acta 178, 195–202 (2012). https://doi.org/10.1007/s00604-012-0810-9

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