摘要
通过优化柱温、流动相、流量等色谱条件,采用高效液相色谱法测定一锅法制备的1-甲基-3,4,5-三硝基吡唑(MTNP)及中间产物1-甲基-4-硝基吡唑(4-MNP)、1-甲基-4,5-二硝基吡唑(4,5-MDNP)、1-甲基-3,5-二硝基吡唑(3,5-MDNP)的含量。反应液经乙腈稀释后,添加适量内标2-硝基甲苯,采用优化的色谱条件测定。以AT.C18色谱柱为固定相,在柱温30℃,流动相体积比45∶55的乙腈和0.1%(体积分数)乙酸溶液的混合溶液,流量1.0 mL·min^(−1)下等度洗脱分离4种目标物,在检测波长265 nm下采用内标法进行定量。结果显示:4种目标物的分离度大于2.5,其质量浓度分别在10.00~250.00 mg·L^(−1)(MTNP和4-MNP)和10.00~350.00 mg·L^(−1)(4,5-MDNP和3,5-MDNP)内和峰面积比值呈线性关系,检出限(3S/N)为0.40~0.80 mg·L^(−1),加标回收率为97.3%~105%,测定值的相对标准偏差(n=6)小于1.0%。
By optimizing chromatographic conditions such as column temperature,mobile phase,and flow rate,l-methyl-3,4,5-trinitropyrazole(MTNP)and intermediate products of 1-methyl-4-nitropyrazole(4-MNP),1-methyl-4,5-dinitropyrazole(4,5-MDNP),and 1-methyl-3,5-dinitropyrazole(3,5-MDNP)prepared by one pot reaction were determined by high performance liquid chromatography.After diluting the reaction solution with acetonitrile,an appropriate amount of internal standard(2-nitrotoluene)was added,and the mixed solution was determined under optimized chromatographic conditions.The AT.C18 chromatographic column was used as the stationary phase.Four targets were separated by isocratic elution at flow rate of 1.0 mL·min^(−1)and column temperature of 30℃,with a mixture of acetonitrile and 0.1%(volume frantion)acetic acid solution at volume ratio of 45∶55 as mobile phase.Quantitative analysis was performed by internal standard method at detection wavelength of 265 nm.It was shown that the resolution of the 4 targets was greater than 2.5,and linear relationships between values of the mass concentration and the peak area ratio were kept in the range of 10.00-250.00 mg·L^(−1)(MTNP and 4-MNP)and 10.00-350.00 mg·L^(−1)(4,5-MDNP and 3,5-MDNP),with detection limits(3S/N)in the range of 0.40-0.80 mg·L^(−1).The spiked recoveries were found in the range of 97.3%−105%,and RSDs(n=6)of the determined values were less than 1.0%.
作者
刘永政
王明亚
庞欣强
赵林秀
曹端林
李永祥
LIU Yongzheng;WANG Mingya;PANG Xinqiang;ZHAO Linxiu;CAO Duanlin;LI Yongxiang(School of Chemical Engineering and Technology,North University of China,Taiyuan 030051,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第6期612-615,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
装备预先研究项目资助
作者简介
刘永政,硕士研究生,研究方向主要为含能材料分析检测;通信联系人:李永祥。liyongxiang@nuc.edu.cn。
