Abstract: An analytical method was developed for the determination of phoxim residue in the muscle of crucian carp, which involved matrix solid-phase dispersion (MSPD) followed by high performance liquid chromatography (HPLC) with diode array detector. Under optimal conditions, 0.5 g tissue sample was dispersed with 1.5 g Florisil and 0.5 g anhydrous sodium sulphate, transferred to a cartridge. The cartridge was eluted with 25 mL acetone-hexane (40:60, v/v). The phoxim was separated on an ODS column (250 mm×4.6 mm, 5 μm) with methanol-water (50:50, v/v) as the mobile phase at the flow rate of 0.6 mL/min, then detected by a diode array detector at 270 nm. The injection volume was 20 μL. The linear range of the method was 0.01~10 mg/L and the detection limit was 3.3 μg/kg. The average recoveries spiked at the levels of 0.05, 0.1, 1 mg/kg ranged from 88% to 112% with the relative standard deviations (RSDs) of 1.1% ~6.3%. The method is quick, simple and can meet the requirement of the analysis of pesticide residues.

Key words: crucian carp , high performance liquid chromatography (HPLC), pesticide, phoxim, residue, matrix solid-phase dispersion (MSPD)