Abstract
Mycotoxins commonly contaminate grains and traditional Chinese medicinal materials, posing serious health risks to humans and animals. To address this issue, a magnetic microporous organic network (MMON) was synthesized via an in situ growth method and Sonogashira-Hagihara coupling for the simultaneous adsorption of seven mycotoxins, followed by UPLC-MS/MS detection. The optimized MMON featured a high surface area, uniform micropores, and rapid magnetic separation within 5 s. Structural and compositional analyses confirmed its tailored architecture, while DFT calculations revealed a pore confinement effect, π-π stacking, and hydrophobic interactions as the primary adsorption mechanisms. A magnetic solid-phase extraction (MSPE) method using 8 mg of MMON achieved adsorption equilibrium within 10 s in 5 mL of a 4 mg/L mycotoxin standard solution. The material maintained over 95% efficiency across ten reuse cycles at a low cost. Under optimal conditions, an MSPE-UPLC-MS/MS method with a low detection limit (0.002-0.15 μg/L), wide linear range (0.01-100.0 μg/L), large enrichment factor (20.1-21.9), low adsorbent dosage, and short extraction time was developed. The determination of mycotoxins in complex grain-based foods and herbal products was also realized with recoveries of 81.32% to 116.10%. This work offers a rapid, cost-effective, and high-throughput approach for mycotoxin detection, supporting quality control in food and herbal product safety.