Magnetic covalent organic framework as a solid-phase extraction absorbent for sensitive determination of trace organophosphorus pesticides in fatty milk

• MSPE based on magnetic COF-DtTb was presented for the analysis of OPPs in fatty milk. • Adsorption mechanisms were demonstrated based on FT-IR and XPS analysis. • The established method without protein precipitation was simple, rapid, and efficient. • Systematic validation proved its high sensitivity and potential application prospect. A simple and efficient magnetic solid-phase extraction (MSPE) method was established with magnetic covalent organic framework (COF) as adsorbent to enrich organophosphorus pesticides from fatty milk samples, followed by the sensitive determination via LC-MS/MS. The key parameters influencing the MSPE efficiency were comprehensively investigated to afford an optimized procedure. All the target analytes could be captured directly by magnetic COF from milk without protein precipitation, making the pretreatment rapid and convenient. Systematic method validation demonstrated its satisfactory linearity, recoveries (80.0-105 %), and precision (RSDs <12.3 %). The method limits of quantification were 0.2-0.5 μg L −1 . A comparison experiment to the reported solid-phase extraction fully verified the present MSPE more rapid, accurate, and environment-friendly. Furthermore, FT-IR and XPS analysis were performed to reveal the adsorption mechanisms of magnetic COF to organophosphorus pesticides, which could offer guidance on the rational design of COF adsorbent for various target analytes.