摘要
为准确测定3,4-二硝基吡唑产品的纯度,建立了3,4-二硝基吡唑及其合成过程中可能存在的杂质(3-硝基吡唑、1,3-二硝基吡唑)的高效液相色谱分析方法。讨论了不同流动相体系、流动相比例、流速等条件对3,4-二硝基吡唑高效液相色谱分离效果的影响。采用外标法进行定量分析。结果表明,得出最优的色谱条件为:Hypersil ODS2色谱柱(250 mm×4.6 mm,5μm),紫外检测波长260 nm,流动相为乙腈/0.1%乙酸水=35∶65(V/V),流速1.0 m L·min^(-1),柱温25℃,进样量10μL。在上述色谱条件下,3-硝基吡唑、3,4-二硝基吡唑和1,3-二硝基吡唑的保留因子分别为0.41、1.20、1.52,3-硝基吡唑和3,4-二硝基吡唑间的分离度为9.42,3-硝基吡唑和1,3-二硝基吡唑间的分离度为3.16。3,4-二硝基吡唑线性范围为5~500 mg·L^(-1),3-硝基吡唑的线性范围为5~250 mg·L^(-1),1,3-二硝基吡唑的线性范围为5~250 mg·L^(-1)。在此范围内,三种化合物的检测限分别为1.19,0.60,1.04 mg·L^(-1),相对标准偏差为1.39%~2.08%,加标回收率为95.29%~103.43%。
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,5μm),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 10μL.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%.
作者
刘圆圆
许建新
王建龙
陈芳
陈丽珍
曹端林
LIU Yuan-yuan;XU Jian-xin;WANG Jian-long;CHEN Fang;CHEN Li-zhen;CAO Duan-lin(School of Chemical Engineering and Environment,North University of China,Taiyuan 030051,China;Gansu Yinguang Chemical Industry Group Co.,Ltd,Baiyin 730900,China)
出处
《含能材料》
EI
CAS
CSCD
北大核心
2018年第2期173-177,共5页
Chinese Journal of Energetic Materials
