高效液相色谱法分析2,6-二氨基-3,5-二硝基吡啶-1-氧化物的纯度  

Purity Analysis of 2,6-Diamino-3,5-dinitropyridine-1-oxide by High Performance Liquid Chromatography

作　　者：张蒙蒙[1] 张林 王友兵[1] 周杰文[1] 李媛[1] ZHANG Meng-meng;ZHANG Lin;WANG You-bing;ZHOU Jie-wen;LI Yuan(Xi’an Modern Chemistry Research Institute,Xi’an 710065,China;Army Representation Office of Air Force in Northwest,Xi’an 710043,China)

机构地区：[1]西安近代化学研究所,陕西西安710065 [2]空军驻西北地区军事代表室,陕西西安710043

出　　处：《火炸药学报》2018年第5期512-516,530,共6页Chinese Journal of Explosives & Propellants

摘　　要：为了分析炸药中主成分2,6-二氨基-3,5-二硝基吡啶-1氧化物(ANPyO)和主要杂质2,6-二氨基-3,5-二硝基吡啶(ANPy)的纯度,建立了高效液相色谱分析方法,该法在岛津InertSustain C18色谱柱(5μm,4.6mm×250mm)进行,以甲醇和水(体积比为40∶60)为流动,相流速为1mL/min,紫外-可见检测器检测波长315nm,柱温30℃,ANPyO用二甲基亚砜溶解,进样量10μL。结果表明,在优化的色谱条件下,ANPyO在质量浓度20～500mg/L范围内线性关系良好,线性相关系数R2为0.997,相对标准偏差RSD≤0.24%。该方法线性范围广,灵敏度高,重现性好,结果准确可靠,可用于ANPyO检测分析,满足实际样品分析的需求。To analyze the purity of main component 2,6-diamino-3,5-dinitropyridine-1-oxide(ANPyO)and main impurity 2,6-diamino-3,5-dinitropyridine(ANPy)in explosive,a high performance liquid chromatography(HPLC)analysis method was established.The method was carried out in InertSustain C18 chromatographic column(5μm,4.6 mm×250 mm),using methanol and water with volume ratio of 40:60 as mobile phase,flow rate as 1mL/min,the detection wavelength of UV-visible detector as 315nm,column temperature as 30℃,dissolution of ANPyO by DMSO,sampling quantity as 10uL.The results show that under the optimized chromatographic conditions,a good linearity with correlation coefficient of 0.997 is obtained in the mass concentration range of 20-500 mg/L.The standard deviation of the method is not greater than 0.24%,indicating that the method has wide linear range,high sensitivity and good reproducibility,and the results are accurate and reliable.It can be applied in the determination of the purity of ANPyO,meeting the needs of actual sample analysis.

关 键 词：高效液相色谱法 2 6-二氨基-3 5-二硝基吡啶(ANPy) 2 6-二氨基-3 5-二硝基吡啶-1氧化物(ANPyO) 二甲基亚砜 纯度 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O647[理学—物理化学]