离子迁移谱定量检测复杂基质中新型炸药六亚甲基三过氧化二胺

摘要

Hexamethylene triperoxide diamine ( HMTD ) , as one kind of new organic peroxide explosives, was often used in the terrorist attacks due to its easy synthesis from available starting materials. Herein, on the basis of nonradioactive ionization source vacuum ultraviolet lamp ( VUV ) , a dopant-assisted positive photoionization ion mobility spectrometer was developed for the determination of HMTD. Toluene and ketones such as acetone, and 2-butanone, were tested as dopants, and acetone was finally chosen as the optimal dopant for the quantitative detection of HMTD in perfume. With mass spectrometer, the reactant ions and the product ions of HMTD were assigned. The reactant ions of acetone were proton dimer m/z 117 [ ( CH3 ) 2 CO] 2 H+, while the product ions of HMTD were proton molecular ion m/z 209 [ HMTD+H]+. When both the drift tube and the thermal desorber temperature was under 120℃, the HMTD standard samples were quantified with the maximum signal intensity and the signal intensity at the 10th second, the linear range was 5-50 ng/μL and 5-100 ng/μL, and the limit of detection ( LOD) was 0. 2 and 0. 3 ng/μL, respectively. Cosmetics such as perfume often interfered and inhibited the measurement of ion mobility spectrometry, so the detection of HMTD in perfume matrix for the rapid screening and detection of HMTD on-site was of realistic significance. These two quantitative methods were used for the quantitative detection of HMTD in three different brands of perfume samples. By comparison, the method using the 10th second signal intensity of HMTD for the quantitative detection had a better recovery and accuracy. This method was suitable for the accurate and rapid quantitative detection of HMTD in complex matrix.%六亚甲基三过氧化二胺( Hexamethylene triperoxide diamine, HMTD)是一种新型有机过氧化爆炸物,由于原料易得、制备方法简单,常被用于恐怖袭击和犯罪活动中。本实验基于非放射性电离源真空紫外灯( VUV)发展了一种试剂分子辅助灯电离正离子迁移谱技术,通过优化筛选试剂分子,最终选择丙酮作为HMTD定量检测的试剂分子。利用质谱对丙酮的反应试剂离子和HMTD的产物离子进行了离子归属,确定反应试剂离子为丙酮二聚体离子 m/z 117[( CH3)2 CO ]2 H+, HMTD 的产物离子为其质子化的分子离子m/z 209[ HMTD+H]+。在迁移管和热解析温度120℃的条件下,利用HMTD最大信号强度和第10 s的信号强度对其标准样品进行定量检测,线性范围分别为5~50 ng/μL和5~100 ng/μL,检出限分别可达0.2和0.3 ng/μL。化妆品如香水等常常干扰和抑制离子迁移谱测量,发展在香水基质中HMTD的现场快速筛查和检测方法具有现实意义。将这两种定量方法应用于3种不同品牌香水样品中HMTD的定量检测,对比发现利用HMTD第10 s的信号强度进行定量具有较好的回收率和准确性,该方法适用于复杂基质中HMTD的准确快速定量检测。