CHINESE JOURNAL OF ENERGETIC MATERIALS
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基于高效液相色谱的BPTAP纯度分析方法
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1.中国工程物理研究院化工材料研究所, 四川 绵阳 621900;2.中北大学环境与安全工程学院, 山西 太原 030051

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国家自然科学基金资助(21975235)


Development of a HPLC Method for the Purity Analysis of BPTAP
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1.Institute of Chemical Materials, CAEP, Mianyang 621900, China;2.School of Environment and Safety Engineering, North University of China, Taiyuan 030051, China

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    摘要:

    高效液相色谱(HPLC)具有灵敏度高、重现性好、分析效率高、自动化程度高等优势,是材料研发过程中纯度分析、质量检测的重要手段之一。四硝基苯并-1,3a,6,6a-四氮杂戊搭烯并吡啶(BPTAP)作为近年来广受关注的一种新型耐热炸药,目前尚缺乏相应的HPLC分析方法。本研究考察并优化了BPTAP的色谱分离条件,建立了基于HPLC的BPTAP纯度分析方法。该方法基于Plus C18色谱柱(4.6×150 mm,5.0 µm),以乙腈-水混合液(含0.1 mg·mL-1乙酸铵)为流动相,采用梯度洗脱模式,检测波长为230 nm。该分析方法下,BPTAP的保留时间为9.13 min,各峰分离度均大于1.90,分离效果良好。进一步对该方法进行验证,BPTAP在0.5~200 µg·mL-1范围内呈良好的线性关系,相关系数R2为0.9997,检测限和定量限分别为0.02 µg·mL-1和0.07 µg·mL-1,并具有良好的精密度、稳定性和耐用性。此外,还将该方法用于BPTAP重结晶过程的纯度检测,结果表明本方法在BPTAP研制过程的含量分析与质量控制中具有良好的应用前景。

    Abstract:

    High performance liquid chromatography (HPLC) has several advantages, such as high sensitivity, good reproducibility, high efficiency, and high automation. HPLC is widely used for purity analysis and quality monitoring of chemical materials. 2,4,8,10-Tetranitrobenzopyrido-1,3a,6,6a-tetraazapentalene (BPTAP) as a new heat-resistant explosive has received wide attentions in recent years. However, there is a lack of HPLC method for BPTAP at present. Thus, we investigated and optimized the chromatographic conditions of separating BPTAP, and established a HPLC method for the analysis of BPTAP purity. The method is based on a Plus C18 column (4.6×150 mm, 5.0 µm) by using the mixture of acetonitrile and water (containing 0.1 mg·mL-1 ammonium acetate) as the mobile phase. Gradient elution mode was used with the detection wavelength at 230 nm. The retention time of BPTAP is 9.13 min with good resolution of all peaks (greater than 1.90). The method was further verified, and it is found that BPTAP has a good linear relationship between 0.5 µg·mL-1 and 200 µg·mL-1 with correlation coefficient (R2) of 0.9997. The detection limit and quantification limit are 0.02 µg·mL-1 and 0.07 µg·mL-1, respectively. In addition, the method was used for the purity analysis of BPTAP after the recrystallization, and it is proved that this method has good performance for the analysis of BPTAP.

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引用本文

丁欢,陈建波,赵海霞,等.基于高效液相色谱的BPTAP纯度分析方法[J].含能材料, 2021, 29(7):658-666. DOI:10.11943/CJEM2020318.
DING Huan, CHEN Jian-bo, ZHAO Hai-xia, et al. Development of a HPLC Method for the Purity Analysis of BPTAP[J]. Chinese Journal of Energetic Materials, 2021, 29(7):658-666. DOI:10.11943/CJEM2020318.

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历史
  • 收稿日期: 2020-12-10
  • 最后修改日期: 2021-04-20
  • 录用日期: 2021-04-12
  • 在线发布日期: 2021-04-20
  • 出版日期: 2021-07-25