Two-dimensional metal-organic framework nanosheets coated solid-phase microextraction Arrow coupled with UPLC-Q-ToF-MS for the determination of three veterinary residues in milk and pork.

• A SPME Arrow-UPLC-Q-TOF-MS method was developed. • The 2D-Ni-MOF material is used for the coating of SPME Arrow. • The 2D-Ni-MOF showed superior extraction capacity to three veterinary drugs. • This method was applied to detect three veterinary drugs in milk and pork. This study presents a method utilizing solid-phase microextraction Arrow (SPME Arrow) combined with ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) for the selective detection of three veterinary drugs-thiabendazole, sulfamethazine, and clenbuterol-in milk and pork. Two-dimensional metal-organic framework nanosheets (2D-MOFs) were employed as coating materials for the SPME Arrow. Three types of 2D-MOFs (Ni, Mn, and Co based) were synthesized and characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and a physical adsorption analyzer. The 2D-MOF coatings were fabricated using the electrospinning technique, with polyacrylonitrile (PAN) serving as the binder. Comparative analysis of the three 2D-MOF coatings revealed that 2D-Ni-MOF was the optimal coating material for the SPME Arrow. Optimization of the coating preparation conditions and SPME procedures included determining the optimal mass ratio of 2D-Ni-MOF to PAN, electrospinning time, and extraction and desorption parameters. Equilibrium extraction was achieved within 60 min, and desorption was completed within 30 min. Subsequently, the 2D-Ni-MOF-SPME Arrow-UPLC-Q-TOF-MS method was established and validated under optimal conditions, demonstrating high precision with inter-day precision ranging from 3.8 % to 9.5 % and intra-day precision ranging from 5.1 % to 11.5 %. The reusability study indicated that the extraction performance of the new SPME Arrow remained consistent after 90 adsorption-desorption cycles. The method exhibited linearity in milk and pork over the ranges of 0.002–5 μg L–1 and 0.01–5 μg L–1, respectively. The detection limits in milk and pork were 0.001–0.004 μg L–1 and 0.003–0.007 μg L–1, respectively. This method demonstrated excellent applicability for determining residues of the three veterinary drugs in milk and pork. [ABSTRACT FROM AUTHOR]