Abstract: Objective: A liquid chromatography-tandem mass spectrometry coupled with immunoaffinity column clean-up method was established for the determination of 8 mycotoxins in aquatic products. Methods: The samples were extracted with acetonitrile water (84:16, V:V), and purified by multifunctional immunoaffinity columns. The chromatographic column was Agilent Proshell 120 SB·C₁₈ column (2.1 mm×100 mm, 2.7 μm). Mobile phase was methanol and 5 mmol/L ammonium acetate (containing 0.1% formic acid), gradient elution. The flow rate was 0.4 mL/min, and the column temperature was 40 ℃. The electrospray was operated in both positive and negative mode at the same time, and the samples were detected by multiple reaction monitoring mode (MRM). Results: The linear relations of the eight mycotoxins were good within the concentration range of 1.0~50.0 ng/mL (R²>0.992). The limits of detection were between 0.05~0.50 μg/kg, and the limits of quantification were between 0.17~1.65 μg/kg. The average recoveries were 75.6%~106.3%, and the relative standard deviations (RSDs) were 3.5%~9.3%. Conclusion: The method is simple, sensitive and accurate for the rapid analysis of mycotoxin residues in aquatic products.