UPLC-Q-TOF/MS快速检验17种有机炸药  

Analysis of 17 Organic Explosives by UPLC-Q-TOF/MS

作　　者：李晓飞[1] 谢伟宏[1] 徐洁蕾[2] LI Xiaofei;XIE Weihong;XU Jielei(Hangzhou Criminal Science and Technology Institute,Hangzhou 310016,China;Hangzhou Normal University,Hangzhou 311121,China)

机构地区：[1]杭州市公安局刑事科学技术研究所,杭州310016 [2]杭州师范大学,杭州311121

出　　处：《刑事技术》2023年第3期300-305,共6页Forensic Science and Technology

基　　金：杭州市农业与社会发展科研项目(2020ZDSJ0425)。

摘　　要：本文建立了超高效液相色谱–四级杆串联飞行时间质谱测定涉爆案件中17种有机炸药(TNT、RDX、HMX、PETN、CE、2-Am-DNT、4-Am-DNT、PYX、2-HADNT、4-HADNT、1,2-DNG、1,3-DNG、3,5-DNA、R-SALT、4-NDPA、NTO、4,4’-DNDPA)的快速定性、定量方法。本研究将有机炸药爆炸残留物或原药经有机溶剂直接溶解,用PLD+净化柱或有机微孔过滤膜净化提取,提取液采用超高效液相色谱–四级杆串联飞行时间质谱进行定性、定量检测。分析采用Shim-pack Velox Biphenyl(2.1 mm×100 mm×2.7μm)色谱柱,质谱扫描方式为负离子的全扫描/数据依赖二级质谱扫描(Full MS/DDA-MS2)模式。结果表明17种有机炸药的检出限在0.1~10 ng/mL之间,所有目标物在其相应的浓度范围内线性关系良好,日内相对标准偏差(RSD)为1.6%~5.3%(n=6),日间相对标准偏差(RSD)为1.7%~8.5%(n=24)。应用本方法可同时准确、快速、高效地对涉爆案件中的17种有机炸药进行定性、定量分析。An analytical method was developed for the simultaneous determination of 17 organic explosives(TNT、RDX、HMX、PETN、CE、2-Am-DNT、4-Am-DNT、PYX、2-HADNT、4-HADNT、1,2-DNG、1,3-DNG、3,5-DNA、R-SALT、4-NDPA、NTO and 4,4’-DNDPA)and its explosive remnants from explosion cases by the ultra-high performance liquid chromatography-quadrupole-time offlight mass spectrometry(UPLC-Q-TOF/MS).The samples were dissolved with the organic solvent,and the solution obtained was purified with a PLD+polymer column or organic microporousfilter membrane.The extract was separated on a Shim-pack Velox Biphenyl column(2.1 mm×100 mm×2.7µm)using acetonitrile–0.05%ammonium chloride as a mobile phase by gradient elution and analyzed under ESI negative ionization Full MS/DDA-MS2 mode.Full scan experiments(TOF/MS&Production)were performed over the m/z range of 40–800 Da.Primary and secondary mass spectrometry information was collected in sequence.The relevant databases about the detected organic explosives was also established.The qualitative screening was performed using Lab Solutions Insight software through a combined score obtained from 4 factors:mass error,retention time error,isotope ratio difference,and library similarity.The quantitative analysis was carried out by extracting peak area with accurate mass.Under the optimal conditions,a good separation and high sensitivity analysis of 17 organic explosives were obtained.We mainly completed the following three parts:(a)We developed Q-TOF high-resolution mass spectrometry for the qualitative analysis and quantification of 17 organic explosives got a fast(10 minutes),high accurate qualitative(resolution 70000 FWHM)detection method.The method was applied to the detection of 17 organic explosives(TNT、RDX、HMX、PETN、CE et al.)and their explosive remnants from explosion cases.(b)The absolute value mass error of this analysis method was below 3.57.The limit of detection(LOD)for 17 organic explosives was 0.1–10 ng/mL.All the compounds had good linearities withi

关 键 词：微量物证 有机炸药 超高效液相色谱–四级杆串联飞行时间质谱 涉爆案件 

分 类 号：D918.9[政治法律—法学] O657.63[理学—分析化学]