Abstract: Sample of mutton was extracted with 0.3 mol·L-1 NaOH solution, after centrifugation, the supernatant was taken and purified by passing through CEC18 solid phase extraction column. The eluate was adjusted to pH 3.0±0.3 with HCl and then further purified by passing through AccuBONDⅡODS-C18 column. The column was eluted with 1.00 mL of 3% (φ) ammoniated methanol and 0.30 mL of water successively. The eluate obtained was used for HPLC analysis. Agilent ZORBAX SB-C18 was used as stationary phase for separation, and a mixture of methanol and water (40+60) was used as mobile phase. The contents of sodium nitrophenolates were determined by UV-detection at the wavelength of 283 nm. Linear relationships between peak area and mass concentration of 3 sodium nitrophenolates were kept in the same range of 50-2 000 μg·L-1. Tests for recovery and precision were tested by addition of 125, 500, 1 000 μg·L-1 of standard solution, and analyzed by the proposed method, giving values of recovery in the range of 74.5%-93.9% and values of RSD′s (n=5) less than 6.5%.