In-coupled syringe assisted octanol–water partition microextraction coupled with high-performance liquid chromatography for simultaneous determination of neonicotinoid insecticide residues in honey

• In-coupled syringe assisted octanol–water partition microextraction as a new method was introduced.
• A couple syringe was used for improving the emulsification.
• No dispersive solvent and centrifugation step was necessary.
• The proposed method is rapid, sensitive and environmental friendly.

A simple and fast method namely in-coupled syringe assisted octanol–water partition microextraction combined with high performance liquid chromatography (HPLC) has been developed for the extraction, preconcentration and determination of neonicotinoid insecticide residues (e.g. imidacloprid, acetamiprid, clothianidin, thiacloprid, thiamethoxam, dinotefuran, and nitenpyram) in honey. The experimental parameters affected the extraction efficiency, including kind and concentration of salt, kind of disperser solvent and its volume, kind of extraction solvent and its volume, shooting times and extraction time were investigated. The extraction process was carried out by rapid shooting of two syringes. Therefore, rapid dispersion and mass transfer processes was created between phases, and thus affects the extraction efficiency of the proposed method. The optimum extraction conditions were 10.00 mL of aqueous sample, 10% (w/v) Na2SO4, 1-octanol (100 µL) as an extraction solvent, shooting 4 times and extraction time 2 min. No disperser solvent and centrifugation step was necessary. Linearity was obtained within the range of 0.1–3000 ng mL−1, with the correlation coefficients greater than 0.99. The high enrichment factor of the target analytes was 100 fold and low limit of detection (0.25–0.50 ng mL−1) could be obtained. This proposed method has been successfully applied in the analysis of neonicotinoid residues in honey, and good recoveries in the range of 96.93–107.70% were obtained.

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