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Triorganotins in seafood are a risks to human health, but due to their low concentrations, their determination is challenging. In this study, a simple and rapid method was developed to isolate triorganotins from seafood by microwave-assisted extraction coupled with magnetic nanoparticle-based purification. The magnetic nanoparticles were coated with octanoic acid. Triethyltin chloride, tributyltin chloride, triphenyltin chloride, and azocyclotin were determined by high performance liquid chromatography– inductively coupled plasma mass spectrometry (HPLC–ICP-MS). Various parameters including the temperature, time, and volume of solvent were optimized to improve the extraction efficiency. Under the optimized conditions, the average recoveries (n = 6) of the triorganotins (fortified at 0.01, 0.02, and 0.05 µg g−1) were between 73.8% and 105.4% and the relative standard deviations were less than 10.4%. The procedure was successfully applied to seafood, and the analytes were measured at concentration levels between 2.93 and 11.26 ng g−1. [ABSTRACT FROM PUBLISHER]