Journal of Food Safety and Quality

Objective To establish a magnetic solid phase extraction (MSPE) approach based on covalent organic framework materials in combination with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the efficient determination of 9 kinds of carbamate pesticides (CPs) in Vigna unguiculata. Methods After the extraction of Vigna unguiculata samples, the novel Fe3O4@TAPOB-BDTB material was employed for magnetic solid-phase extraction and purification. After filtration, the samples were separated by a C18 chromatographic column and quantitatively analyzed using multiple reaction monitoring in the electrospray positive ion mode. Results The established analytical methods for the 9 kinds of CPs exhibited excellent linearity within the concentration range of 0.02–100.00 μg/kg, with the determination coefficients (r2) all exceeding 0.9989. The spiked recovery rates were within the range of 80.33%–108.63%, and both the intra-day and inter-day precisions were less than 8.89%. The detection limits of the methods were 0.005–0.010 μg/kg, and the limits of quantitation were 0.02 μg/kg, which were significantly below the maximum residue limits specified in GB 2763—2021 National food safety standard-Maximum residue limits of pesticides in food and EU Regulation No 396/2005, ensuring compliance within an academic context. Conclusion The covalent organic framework materials synthesize in this study demonstrate exceptional adsorption capacity for CPs via π-π interactions and hydrogen bonding. Furthermore, the develope MSPE-HPLC-MS/MS method enables rapid, highly sensitive, and precise detection of CPs in Vigna unguiculata, thereby offering an efficient and innovative approach for monitoring pesticide residues in agricultural products.

covalent organic framework materials; high performance liquid chromatography-tandem mass spectrometry; carbamate pesticides; magnetic solid phase extraction