Cucurbit[7]uril-assisted matrix solid-phase dispersion coupled with deep eutectic solvent-based dispersive liquid-liquid microextraction for HPLC analysis of neonicotinoid residues in plant foods.

A novel analytical method combining cucurbit[7]uril-based matrix solid-phase dispersion (MSPD@Q[7]) with deep eutectic solvent dispersive liquid-liquid microextraction (DLLME@DES) was developed for extracting four neonicotinoid insecticides from plant foods, followed by HPLC-DAD analysis. Key parameters were screened by one-variable-at-a-time and optimized through Plackett-Burman design and central composite design response surface methodology. The developed method displayed a linear range of 0.2-20 μg/g and R2 values >0.9978 for all four calibration curves. High sensitivity was achieved, as reflected by LODs of 0.007-0.019 μg/g. Method accuracy and precision were confirmed by satisfactory recoveries (81.4-118.8%) and low relative standard deviations (2.1-6.5%) across all matrices, respectively. Extraction mechanisms were elucidated via various experimental techniques and molecular dynamics simulations. Greenness assessment using AGREEprep and BAGI tools confirmed the method's environmental advantages, including solvent-free operation and minimal matrix effects. This approach provides a sensitive, eco-friendly solution for neonicotinoid residue analysis in complex plant food matrices.