Abstract: HPLC was applied to the simultaneous determination of tetramethrin and d-phenothrin using Hypersil C18 stainless steel chromatographic column and the mobile phase of acetonitrile-water (85+15) mixture for separation, and UV-detection at the wavelength of 220 nm in the determination. The proposed method was feasible to be used for control analysis of the compound insecticide 0.3% tetramethrin·d-phenothrin aerosol. Values of RSD′s (n=5) found were 0.86% for tetramethrin and 2.6% for d-phenothrin, and values of recovery found were in the ranges of 94.7%-105.5% and 92.8%-102.9% respectively.