Abstract: A reverse phase high performance liquid chromatography method was developed for determination of hydrogen cyanide in cigarette mainstream smoke via metal-complexing derivatization. By using Ni(II)-NH₃ as derivatizating agent, the proposed method can achieve the analysis within 10 minutes using 5 mmol/L tetraamylammonium bromide as ion-pair reagent. The method enabled good linearity in the range from 0.1 to 20 μg/mL for the standard working solutions with R² higher than 0.999. The limit of detection and limit of quantization were 0.049 μg/cig and 0.162 μg/cig, respectively. The recoveries for spiked samples at three levels were between 87.41% and 119.47%. The test results of the proposed method were in good agreement with that of continuous flow method with a relative deviation of -5.35% for Kentucky reference cigarette 3R4F and a relative deviation range from -0.79% to 8.51% for 15 cigarette samples.