[Application of matrix solid-phase dispersion for the determination of phoxim in crucian carp samples by high performance liquid chromatography].
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.
Liu
Qian
Q
College of Food Science and Technology, Huazhong Agricultural University, Wuhan, China.
Liu
Xiaoyu
X
Qiu
Chaokun
C
Wang
Xiaobao
X
Ren
Hongmin
H
D000818:Animals; D002347:Carps; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D009946:Organothiophosphorus Compounds / Q000032:analysis*; D010573:Pesticide Residues / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods*
D009946:Organothiophosphorus Compounds; D010573:Pesticide Residues; C003135:phoxim