A method for determination of pyrethroid insecticide residues in fruits and vegetables based on a simple extraction using acetonitrile followed by solid-phase extraction and high-performance liquid chromatography-UV is described. Separation of pyrethroids was carried out on an Atlantis C18 column using an isocratic mobile phase of 75% acetonitrile with a flow rate of 1.0 mL min−1 and UV detection at 225 nm. Matrix effect was overcome using matrix-matched standards for building up the calibration graphs. The linear ranges were established between 0.01 and 0.50 μg mL−1. The concentration of pyrethroids was enhanced with the factors up to 1,025 folds. The method has been successfully applied in a monitoring of pyrethroid residues contaminated in fruits and vegetables.