The unreasonable use of organophosphorus pesticides leads to excessive pesticide residues in food, seriously threatening public health, and the potential of surface-enhanced Raman spectroscopy (SERS) technology, incorporating a metal–organic framework, is substantial for the rapid detection of trace pesticide residues. Here, a novel Fe 3 O 4 @NH 2 -MIL-101(Fe)@Ag (FNMA) SERS nanosensor was developed. Results indicated that the FNMA had a high enhancement factor of 1.53 × 10 8 , a low limit of detection (LOD) of 4.55 × 10 −12 M, and a relative standard deviation of 7.73 % for 4-nitrothiophenol, demonstrating its good SERS sensitivity and uniformity, and also possessed good storage stability for one month. In quantifying fenthion and methyl parathion in standard solutions and apple juice in the range of 0.05/0.02–20 mg/L, it showed LODs of 3.02 × 10 −3 mg/L and 1.43 × 10 −3 mg/L, and 0.0407 and 0.0075 mg/L, respectively, demonstrating potentials in ultrasensitive trace detection of pesticides in food.
An acryloyl β-cyclodextrin-silica hybrid monolithic column for pipette tip solid-phase extraction and high-performance liquid chromatography determination of methyl parathion and fenthion has been prepared through a sol–gel polymerization method. The synthesis conditions, including the volume of cross-linker and the ratio of inorganic solution to organic solution, were optimized. The prepared monolithic column was characterized by thermogravimetric analysis, scanning electron microscopy, and Fourier transform infrared spectroscopy. The eluent type, volume and flow rate, sample volume, flow rate, acidity, and ionic strength were optimized in detail. Under the optimized conditions, a simple and sensitive pipette tip solid-phase extraction with high-performance liquid chromatography method was developed for the determination of methyl parathion and fenthion in lettuce. The method yielded a linear calibration curve in the concentration ranges of 15–400 μg/kg for methyl parathion and 20–400 μg/kg for fenthion with correlation coefficients of above 0.9957. The limits of detection were 4.5 μg/kg for methyl parathion and 6.0 μg/kg for fenthion, respectively. The recoveries of methyl parathion and fenthion spiked in lettuce ranged from 96.0 to 104.2% with relative standard deviations less than 8.4%.
危险品化学品经营许可证（带存储）