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3,4-二硝基吡唑纯度的高效液相色谱分析方法
Purity Analysis of 3,4-Dinitropyrazole by High Performance Liquid Chromatography
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中文摘要:
      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, 5 μm), 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 mL·min-1, 柱温25 ℃, 进样量10 μL。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%。
中文关键词: 3,4-二硝基吡唑  3-硝基吡唑  1,3-二硝基吡唑  高效液相色谱法(HPLC)  外标法
英文摘要:
       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%.
英文关键词: 3,4-dinitropyrazole  3-nitropyrazole  1,3-dinitropyrazole  high performance liquid chromatography(HPLC)  external standard method
DOI:10.11943/j.issn.1006-9941.2018.02.011
投稿日期:2017-08-01
最后修改日期:2018-01-16
网络出版日期:2018-02-11
书版出版日期:2018-02-12
引用文献:刘圆圆,许建新,王建龙,等.3,4-二硝基吡唑纯度的高效液相色谱分析方法[J].含能材料,2018,26(2):173~177.LIU Yuan-yuan,XU Jian-xin,WANG Jian-long,et al. Purity Analysis of 3,4-Dinitropyrazole by High Performance Liquid Chromatography[J]. Chinese Journal of Energetic Materials(Hanneng Cailiao),2018,26(2):173-177.
作者单位E-mail
刘圆圆 中北大学化工与环境学院, 山西 太原 030051 779530582@qq.com,wangjianlong@nuc.edu.cn,f_chen@nuc.edu.cn 
许建新 甘肃银光化学工业集团有限公司, 甘肃 白银 730900  
王建龙 中北大学化工与环境学院, 山西 太原 030051 wangjianlong@nuc.edu.cn,f_chen@nuc.edu.cn 
陈芳 中北大学化工与环境学院, 山西 太原 030051 wangjianlong@nuc.edu.cn,f_chen@nuc.edu.cn 
陈丽珍 中北大学化工与环境学院, 山西 太原 030051  
曹端林 中北大学化工与环境学院, 山西 太原 030051  
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