Abstract: The freshwater mussel samples were extracted with ethyl acetate solvent.Then the samples were purified by solid-phase extraction with Florisil column.After filtration,the filtrate was concentrated with nitrogen and concentrated with n-hexane.The content was determined by gas chromatography-mass spectrometry(GC-MS) with isotope internal standard method.The results showed that:PAEs had a good linear relationship between 0.10~2.00 mg/L,while the correlation coefficient r² were all above 0.99.The average recoveries ranged from 73.1% to 94.3% with RSD that less than 9.3% by three level of spiked concentrations.The limit of detection were ranged from 1.2 to 3.9 μg/kg.The method had the advantages of simple pretreatment,high sensitivity and high accuracy,and could be satisfied in requirement of detecting phthalate residues in freshwater mussel meat.