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Solid-Phase Extraction Combined with Dispersive Liquid–Liquid Microextraction for the Simultaneous Determination of Deltamethrin and Permethrin in Honey by Gas Chromatography–Mass Spectrometry

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Abstract

In this study, solid-phase extraction combined with dispersive liquid–liquid microextraction is presented for the simultaneous determination of trace amounts of deltamethrin and permethrin in honey by gas chromatography–mass spectrometry. First, permethrin and deltamethrin were extracted from polluted honey samples by ultrasound-assisted liquid–liquid extraction followed by solid-phase extraction (SPE). Then, the analytes were eluted from the SPE cartridge. The elution solvent containing trace amounts of analytes was applied in dispersive liquid–liquid microextraction (DLLME) step as disperser solvent for further purification and preconcentration of deltamethrin and permethrin. The important parameters such as the type and volume of the solvent for initial extraction of pesticides from honey matrix, the amount of honey, and type and volume of extraction solvent and elution solvent (disperser solvent) were investigated through the process. Under the optimal conditions, good linearity in the range of 0.2–800 ng g−1 with the correlation coefficient (r 2) >0.9986 and 0.9990, low limits of detection (LODs) of 0.02 and 0.04 ng g−1, enrichment factors of 4955 and 4925, and relative standard deviations (RSD%, n = 7) of 1.8 and 2 % were obtained for permethrin and deltamethrin, respectively. The proposed procedure showed satisfactory results for simultaneous determination of deltamethrin and permethrin in honey. Relative recoveries of 94–99.2 % were obtained for real sample analysis.

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Acknowledgments

The financial support of this project by Shahrekord University and Isfahan Payame Noor University is appreciated. The authors were also partially supported by the Center of Excellence for Mathematics, Shahrekord University.

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Authors and Affiliations

  1. Department of Chemistry, Faculty of Sciences, Shahrekord University, P.O. Box 115, Shahrekord, Iran

    Mahboube Shirani, Hedayat Haddadi & Abolfazl Semnani

  2. Nuclear Fuel Cycle Research School, Nuclear Science & Technology Research Institute, Atomic Energy Organization of Iran, P.O. Box 14395-836, Tehran, Iran

    Mohammad Rezaee

  3. Department of Chemistry, Payame Noor University, P.O. Box 19395-4697, Tehran, Iran

    Saeed Habibollahi

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  1. Mahboube Shirani
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  2. Hedayat Haddadi
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Correspondence to Hedayat Haddadi.

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No conflict exists; author Mahboube Shirani declares that she has no conflict of interest. Author Hedayat Haddadi declares that he has no conflict of interest. Author Mohammad Rezaee declares that he has no conflict of interest. Author Abolfazl Semnani declares that he has no conflict of interest. Author E Saeed Habibollahi declares that he has no conflict of interest.

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Shirani, M., Haddadi, H., Rezaee, M. et al. Solid-Phase Extraction Combined with Dispersive Liquid–Liquid Microextraction for the Simultaneous Determination of Deltamethrin and Permethrin in Honey by Gas Chromatography–Mass Spectrometry. Food Anal. Methods 9, 2613–2620 (2016). https://doi.org/10.1007/s12161-016-0455-0

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