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Determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons by HPLC following sample clean-up by ion-pairing

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Abstract

An efficient analytical method is presented involving effective sample clean-up with solid-phase extraction and HPLC-UV analysis for the simultaneous determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons. Sample preparation involves extraction with acetonitrile acidified with trifluoroacetic acid and an ethyl acetate/petroleum ether mixture. Purification of the crude extract was carried out with liquid–liquid partitioning after addition of an aqueous ammonia solution. Final clean-up was performed on polymeric reversed-phase cartridges pretreated with sodium dodecyl sulfate. Chromatographic analysis was performed on a reversed-phase HPLC column isocratically eluted with an acetonitrile/water/ammonia mixture and UV detection at 254 nm. The chromatographic method is repeatable, reproducible, and sensitive. Fungicide recoveries from lemon samples fortified at levels of 5 and 1 mg kg−1 were 81–85% for carbendazim, 96–98% for thiabendazole, and 81–106% for o-phenylphenol with coefficients of variation of 2.5–7.4%. Detection limits for carbendazim, thiabendazole, and o-phenylphenol in lemons were 0.21, 0.27, and 0.51 mg kg−1, respectively.

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Authors and Affiliations

  1. Department of Chemistry, Section of Organic Chemistry, Biochemistry and Natural Products, University of Patras, 26500, Patras, Greece

    Konstantinos P. Prousalis, Dimitris A. Polygenis, Alexandra Syrokou, Fotini N. Lamari & Theodore Tsegenidis

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  1. Konstantinos P. Prousalis
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  2. Dimitris A. Polygenis
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  3. Alexandra Syrokou
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  4. Fotini N. Lamari
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  5. Theodore Tsegenidis
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Correspondence to Theodore Tsegenidis.

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Prousalis, K.P., Polygenis, D.A., Syrokou, A. et al. Determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons by HPLC following sample clean-up by ion-pairing. Anal Bioanal Chem 379, 458–463 (2004). https://doi.org/10.1007/s00216-004-2614-1

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  • DOI: https://doi.org/10.1007/s00216-004-2614-1

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