ASE-HPLC检测某型号球形发射药中的叠氮硝胺、硝化甘油、Ⅱ号中定剂含量的研究

Determination of the Components in the Globule Gun-propellant Using Accelerated Solvent Extraction(ASE) Followed by HPLC

采用快速溶剂萃取（ASE）技术和高效液相色谱法测定某球形药中叠氮硝胺（DIANP）、硝化甘油（NG）和Ⅱ号中定剂（C2）的含量．ASE提取条件：二氯甲烷做萃取溶剂，萃取温度100℃，静态萃取10min，萃取2次．HPLC测定条件：YWGC18柱（150×4．6mm，10μm），以甲醇和水作为流动相，梯度洗脱，流速1 mL／min，检测波长210nm．测定结果表明DIANP、NG、C2平均回收率分别为99．6％、100．3％、99．4％，RSD分别为0．7％、0．8％、0．9％（n=5），检出限分别为2.1、1.5和0．2mg／L，线性范围分别为0．02～0．98g／L，0．03～1．38g／L，0．002～0．124g／L．用此方法共检测某批球形发射药样品5份，检测结果与滴析-HPLC法检测结果相当．

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,10μm） 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.