Abstract: HPLC was applied to the determination of residual amount of phoxim in feed. The sample was extracted with ethyl acetate and purified by passing through NH2-solid phase extraction column. Reverse C18 chromatographic column was used as stationary phase, and a mixed solution of acetonitrile and water (65+35) was used as mobile phase. UV-detection at 280 nm was adopted in the determination. Linear relationship between values of peak area and mass concentration of phoxim was obtained in the range of 0.10-0.50 mg·L-1, with detection limit of 0.10 mg·kg-1. Values of recovery found by standard addition method were in the range of 80.0%-88.2%, and values of RSD′s (n=5) in the range of 1.6%-6.5%.