To accurately determine the purity of 3, 4-dinitropyrazole product, a high performance liquid chromatography (HPLC) method for the determination of 3, 4-dinitropyrazole and possible impurities, 3-nitropyrazole and 1, 3-dinitropyrazole, occurring in its synthetic process was established. The effect of different mobile phase system, mobile phase ratio and flow rate etc. conditions on the separation effect of high performance liquid chromatography for 3, 4-dinitropyrazole was discussed. The quantitative analysis was carried out by an external standard method. Results show that The optimal chromatographic conditions obtained are as follows: hypersil ODS2 chromatographic column (250 mm×4.6 mm, 5 μm), UV detection wavelength 260 nm, acetonitrile/0.1% acetic acid with a volume ratio of 35:65 as mobile phase, flow rate 1.0 mL·min^-1, column temperature 25 ℃, injection volume 10 μL. Under the above-mentioned conditions, the retention factors of 3-nitropyrazole, 3, 4-dinitropyrazole and 1, 3-dinitropyrazole are 0.41, 1.20, 1.52, respectively. The resolution between 3-nitropyrazole and 3, 4-dinitro-pyrazole is 9.42, and the resolution of 3-nitropyrazole with 1, 3-dinitrazole is 3.16. 3, 4-Dinitropyrazole, 3-nitropyrazole and 1, 3-dinitropyrazole show a good linear relationship in the concentration range of 5-500 mg·L^-1, 5-250 mg·L^-1 and 5-250 mg·L^-1, respectively. The detection limits of 3, 4-dinitropyrazole, 3-nitropyrazole and 1, 3-dinitropyrazole are 1.19, 0.73, 1.04 mg·L^-1, respectively. The standard recovery rates are 98.17%-104.84% with the relative standard deviations of 1.39%-2.08%.