Abstract: To achieve rapid and sensitive detection of six carbamate pesticides (CPs) in vegetables, this study developed a high-efficiency solid-phase extraction (SPE) coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method based on a novel polyether sulfone/polydopamine/covalent organic framework composite membrane. The results showed that the composite membrane was fabricated using a polyether sulfone membrane as the substrate and polydopamine as the intermediate layer. A pre-anchored aldehyde monomer, 2,5-dihydroxy-1,4-benzenedicarboxaldehyde, was employed to achieve the in-situ growth of the covalent organic framework on the membrane surface, significantly enhancing the adsorption performance and selectivity of the composite membrane. Under optimized SPE conditions, the method demonstrated excellent analytical performance: in head cabbage, cucumbers, and Chinese cabbage, it showed relatively low matrix effects (−8.26% to 10.74%), with limits of detection (LOD) of 0.008–0.050 μg/kg and limits of quantification (LOQ) of 0.027–0.167 μg/kg. Recoveries from spiked ranged from 82.47% to 105.57%, with relative standard deviations (RSDs) less than 6.0%, indicating excellent accuracy and precision. The prepared composite membrane had good purification capacity and reusability, greatly reducing matrix interference and operational complexity. This method provides an efficient and reliable technical platform for routine monitoring of trace CPs in vegetables, holding broad application prospects.

Key words: high performance liquid chromatography-tandem mass spectrometry; covalent organic framework; composite membrane; solid phase extraction; carbamates; pesticide residues