Rapid determination of chlorpyrifos and fluvalinate in mixed insecticide was established by using high performance liquid chromatography. Result were as follows : 1. On Lichrosorb${circledR}$ RP-8(10 ${mu}m$) Column with on fluent of acetanitrile : water=75 . 25, sufficient separation of Chlorpyrifos and Fluorinate of base was obtained. 2.410td portion the diluted solution was injected in to the cdumn, and the effluent was monitored by on UV-Detector at 270 nm. 3. Relative Standard Deviation were 0.97% (chlorpyrifos) and 0.5% (fluorinate) under analysis conditions. 4. The UV-Detector response at 270 nm were linear (Y=421.8X-2090, $R^2=0.9997$ : Chlorpyrifos, Y= 1062.7X-4017.7, $R^2=0.9998$ : Fluorinate) over a range of 30~500 ${mu}g/ml$.