[Application of matrix solid-phase dispersion for the determination of phoxim in crucian carp samples by high...

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 x 4.6 mm, 5 microm) 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 microL. The linear range of the method was 0.01 - 10 mg/L and the detection limit was 3.3 microg/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.