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

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.