Tralomethrin quickly changes to deltamethrin in gas chromatograph by debromination. Therefore deltamethrin and tralomethrin are not able to be distinguished by gas chromatographic determination. A method for specific determination of deltamethrin and tralomethrin was established. The method consists of fractionation by high performance liquid chromatography and determination by gas chromatography. Recoveries of deltamethrin and tralomethrin spiked to three agricultural products were from 42 to 78% and from 18 to 76%, respectively with relative standard deviations ranging from 0.3 to 15%. From the analysis of samples spiked with tralomethrin, it was found that a part of tralomethrin quickly changed to deltamethrin in homogenate of agricultural products. The addition of phosphoric acid to the homogenate did not prevent the change of tralomethrin.