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Ultrasound-assisted solvent extraction (UASE) combined with dispersive liquid–liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) has been developed for extraction and determination of fenvalerate from tomato samples. Fenvalerate was determined by high-performance liquid–liquid chromatography-ultraviolet detector. Effects of parameters such as type and volume of extraction solvent in the UASE stage, sonication time, type and volume of extraction solvent and disperser solvent in the DLLME-SFO stage, salt addition and pH effect on extraction were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 5–500 µg kg −1  with a detection limit of 0.6 µg kg −1 . The relative standard deviation for five replicate measurements of 100 µg kg −1  of fenvalerate was 6.5%. The relative recovery of fenvalerate in different tomato samples at a spiking level of 10, 20 and 50 µg kg −1  is in the range of 93.5–108%. The obtained results show that UASE–DLLME-SFO is a sensitive, fast and simple method for the determination of fenvalerate in tomato samples.

Determination of Fenvalerate in Tomato by Ultrasound-Assisted Solvent Extraction Combined with Dispersive Liquid–Liquid Microextraction