Integration of Carboxylate Mesoporous Silica–Coated Solid Phase Microextraction Arrow and Portable Mass Spectrometer for Simultaneous Determination of Five Veterinary Drugs in Chicken and Milk

A new solid-phase microextraction (SPME) Arrow device was fabricated using mesoporous silica (MCM-41) as the coating material and integrated with a portable mass spectrometer (PMS) to develop a sensitive and selective method for the detection of amantadine, thiabendazole, sulfadimethoxine, clenbuterol, and ractopamine in milk and chicken samples. The influence of different functional groups on the extraction performance of MCM-41 was investigated by synthesizing amine-, vinyl-, and carboxyl-modified MCM-41, representing basic, neutral, and acidic surface properties. Among these, the carboxyl-modified MCM-41 (MCM-41-C) exhibited the highest selectivity and adsorption capacity, attributed to its strong electrostatic interactions and hydrogen bonding with the analytes. The MCM-41-C-SPME Arrow was fabricated using electrospinning to produce a uniform, stable coating, which was then systematically optimized for key extraction and desorption parameters. This novel SPME Arrow-PMS platform enables rapid detection of five analytes within 30 s, with a broad linear range (5–1000 μg kg^–1) and low limits of detection (1.6–30.6 μg kg^–1). The developed method demonstrated excellent intra-day and inter-day reproducibility (RSD < 12%) and high recovery (82–117%). This method offers rapid, sensitive detection of multiple veterinary drugs in complex food matrices, providing a practical solution for on-site food safety monitoring.