Abstract: Objective: to establish the method for determining the components in globule gun-propellant samples. Method: the samples were extracted by ASE200 and determinated by HPLC with UV detection. Parameters such as solvent, temperature, pressure and time were investigated thoroughly. The ASE conditions were as follows: dichloromethane, 100 ℃ and two 10 min cycles were chosen as the extraction solvent, the temperature and time, respectively. The HPLC separation was performed on a YWG C₁₈ column (150×4.6 mm，10 μm) with methanol and water as the mobile phase at a flow rate of 1.0 mL/min. The detection wavelength was 210 nm. Results: the average recovery of DIANP, NG and C₂ were 99.6％, 100.3％ and 99.4％, with a RSDof 0.7％,0.8％ and 0.9％ (n=5). The limits of detection were 2.1 mg/L、1.5 mg/L、0.2 mg/L , respectively. The linear range were 0.02~0.98 g/L, 0.03~1.38 g/L, 0.002~0.124 g/L, respectively. The method was applied to one samples for 5 times.