A high-performance liquid chromatographic(HPLC) procedure for determining AY was described.The method was based on a reversed-phase column(Agilent Hypersil ODS column,125 mm×4.6 mm×5 μm) with precolumn derivatization withο-phthaldialdehyde and fluorometric detection(excitation wave length was 340 nm and emission wave length was 450 nm).AY were separated using gradient solution with the flow rate 1.0 mL /min.It allowed simultaneous determination of AY,free amino acids and other peptides in 30 min.Linearity for each amine was observed from 0.1 to 1 000.0 mg/L.Detection limit was 0.005 mg/L.The average recovery of AY from corn oligopeptides was 97.8%.The method was simple,fast,and reliable.It could be used to detect AY in corn oligopeptides.