CHINESE JOURNAL OF ENERGETIC MATERIALS
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高效液相色谱法检测多硝基金刚烷
作者:
作者单位:

(1. 北京理工大学化工与环境学院, 北京 100081; 2. 南京理工大学化工学院, 江苏 南京 210094)

作者简介:

董学敏(1989-),女,硕士研究生,主要从事色谱分析研究。e-mail: dongxuemin525@163.com 通信联系人: 薛敏(1973-),女,博士,研究生导师,主要从事高分子材料制备及色谱分析研究。e-mail: minxue@bit.edu.cn

通讯作者:

薛敏(1973-),女,博士,研究生导师,主要从事高分子材料制备及色谱分析研究。e-mail: minxue@bit.edu.cn

基金项目:

国家大学生科技创新计划,北京理工大学化工类研究生创新平台资助


Determination of Polynitroadamantanes by HPLC
Author:
Affiliation:

(1. School of Chemical Engineering & the Environment, Beijing Institute of Technology, Beijing 100081, China; 2. School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China)

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    摘要:

    多硝基金刚烷类化合物是合成药物和含能材料重要的前体。建立了2, 2-二硝基金刚烷及2, 2, 4, 4, 8, 8-六硝基金刚烷的高效液相色谱分析方法, 并讨论了不同检测器、流动相、色谱柱等条件对二者分离的影响, 得到二者的最佳分离色谱条件:色谱柱, DIONEX C18 (5 μm, 120 A, 4.6 mm×250 mm), 流动相为乙腈/水(80 /20, V/V), 流速为1.0 mL·min-1, 柱温25 ℃, 检测器为紫外检测器, 检测波长为220 nm。采用上述方法, 得到2, 2-二硝基金刚烷检测限为0.003 mg·mL-1, 线性范围为0.005~1.000 mg·mL-1, 线性相关系数0.9987, 精密度是1.382%; 2, 2, 4, 4, 8, 8-六硝基金刚烷检测限为0.001 mg·mL-1, 线性范围为0.005~1.000 mg·mL-1, 线性相关系数0.9984, 精密度是1.300%。

    Abstract:

    Polynitroadamantanes are the precursors both in pharmaceutical synthesis and energetic material preparation. In this paper, the determination method of 2, 2-nitroadamantane and 2, 2, 4, 4, 8, 8-hexanitroadamantane was established by High Performance Liquid Chromatography (HPLC) with optimal chromatographic conditions including the detector, mobile phase and stationary phase. The Ultraviolet detector and DIONEX C18 column (5 μm, 120 A, 4.6 mm×250 mm) were confirmed to get base line separation and high limit of detection for these two compounds mixture. The acetonitrile/water (80/20, V/V) was employed as mobile phases, which presented exceptional separation effect on these two targets when the flow rate was 1.0 mL·min-1. Results show that the detection limit, linear range, the linear correlation coefficient and precision of 2, 2-nitroadamantane are 0.003 mg·mL-1, 0.005-1.000 mg·mL-1, 0.9987 and 1.382%, respectively. Correspondingly, the same parameters of 2, 2, 4, 4, 8, 8 -hexanitroadamantane are 0.001 mg·mL-1, 0.005-1.000 mg·mL-1, 0.9984 and 1.300%, respectively

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引用本文

董学敏,薛敏,徐志斌,等.高效液相色谱法检测多硝基金刚烷[J].含能材料, 2015, 23(5):450-453. DOI:10.11943/j. issn.1006-9941.2015.05.009.
DONG Xue-min, XUE Min, XU Zhi-bing, et al. Determination of Polynitroadamantanes by HPLC[J]. Chinese Journal of Energetic Materials, 2015, 23(5):450-453. DOI:10.11943/j. issn.1006-9941.2015.05.009.

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  • 收稿日期: 2014-02-26
  • 最后修改日期: 2014-09-17
  • 录用日期: 2014-07-10
  • 在线发布日期: 2015-04-16
  • 出版日期: 2015-04-10