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The paper describes an efficient method for the determination of nitrophenolate sodium in aquatic products by HPLC combined with atmospheric pressure chemical ionization with tandem mass spectrometry (LC-APCI-MS/MS). Analytes were extracted from aquatic products by acetonitrile, the extracts were degreased by alumina and concentrated, the concentrated solution was further purified by Oasis HLB cartridge. Finally, the analytes were separated and detected by LC-APCI-MS/MS in negative ion mode. Excellent linearity with correlation coefficients of more than 0.995 was observed in the concentration range of 2-200 mu g/L for p-nitrophenol sodium and 2-methoxy-5-nitrophenolate sodium, and 5-200 mu g/L for omicron-nitrophenol sodium. Recovery rates of nitrophenolate sodium between 86.1-94.3% were achieved. Limit of quantitation of p-nitrophenol sodium and 2-methoxy-5-nitrophenolate sodium was 2 mu g/kg and omicron-nitrophenol sodium was 5 mu g/kg, with relative standard deviations < 10%. This method was employed in the practical analysis of spiked and naturally contaminated aquatic products.