A new application of high pressure liquid chromatography for the determination of fenitrothion and cis- and trans-neopynamin in insecticidal preparations was investigated. Optimum conditions for a good separation and determination were determined; solvent system: dichloromethane + n-hexane = 17 + 83; Bow rate: 0.5ml/min; column: u-porasil ($4mm{ imes}3Ocm$); absorbance wavelength: 254nm; 0.05 AUFS and sample size: 30 ul. Recovery of fenicrothion, cis- and trans-neopynamin from mixed artificial preparations was 99.6%, 99.7% and 99.8% respectively. Also reproducibility tests showed that the coefficient of variation was 0.89% for fenitrothion, 0.74% cis-neopynamin and 1.1% for trans-neopynamin. There was no interference with insecticidal preparation containing DDVP, allethrin, S-421 and kerosene. HPLC method was rapid, accurate and it gave better reproducibility and higher sensitivity than any other analytical method. It was considered that HPLC could be greatly applied to the analysis of fenitrothion and neopynamin in insecticidal preparations.