Magnetic Fe3O4@SiO2@β-cyclodextrin for solid phase extraction of methyl parathion and fenthion in lettuce samples†

Abstract

In this study, magnetic Fe₃O₄@SiO₂@β-cyclodextrin copolymerized microparticles were synthesized and applied for the extraction of methyl parathion and fenthion in lettuce samples followed by HPLC-UV detection. The magnetic β-cyclodextrin copolymerized microparticles were prepared by dispersion polymerization with acryloyl β-cyclodextrin as the functional monomer and ethylene glycol dimethyacrylate as the crosslinker. The composite magnetic microparticles were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, magnetic measurement, and thermogravimetric analysis, and used as the adsorbent of magnetic solid-phase extraction (MSPE) for methyl parathion and fenthion. The extraction conditions including sample pH and ionic strength, desorption solvent type and volume, and adsorption and desorption times were optimized. Under the optimal extraction conditions, an MSPE-HPLC-UV method was developed for the detection of methyl parathion and fenthion in lettuce. Wide linear ranges of 1.0–200 μg kg^?1 (R² = 0.9998) for methyl parathion and 1.5–200 μg kg^?1 (R² = 0.9978) for fenthion were obtained and the limits of detection were 0.3 μg kg^?1 for methyl parathion and 0.5 μg kg^?1 for fenthion in lettuce, respectively. The proposed method was applied for the determination of methyl parathion and fenthion in lettuce with satisfactory recoveries between 89.2–101.2%, and relative standard deviations were less than 9.1%. Thus, the MSPE-HPLC-UV method has high accuracy and sensitivity for the analysis of methyl parathion and fenthion in lettuce samples.