ase（快速溶剂萃取）-gpc（凝胶渗透色谱净化）-液相色谱质谱-apci .docVIP

LC/APCI/MS对粉尘中炸药成分的分析及应用研究 宣 宇1,2,孙楠1,傅得锋2,郑一平2,莫卫民1,徐晟捷2 1（浙江工业大学化学工程与材料学院，杭州310014） 2（浙江省公安物证鉴定中心，杭州310009） 摘要：高选择性和灵敏度的LC/APCI-MS/MS方法被用来定量分析粉尘样品中的HMX、RDX、PETN、CE、NQ、TNT这6种高能炸药。采用ASE萃取，GPC净化浓缩作为前处理方法，在粉尘中分别添加所测炸药组分，使用丙酮作为ASE萃取溶剂，乙酸乙酯：环己烷（1:1）作为GPC净化时的流动相并抛弃杂质500s，收集1020s。在仪器分析时，通过在流动相中添加1mmol/L甲酸与样品形成[M+HCOO]-的甲酸加合离子。实验测得HMX、RDX、PETN、CE、NQ、TNT的方法检测限分别为0.78，1.44，1.69，0.77，1.06，1.72ng/ml，回收率在49.0%~88.4%之间，相对标准偏差在3.5%~10.3%之间，证明方法可以用来系统排查及定量分析爆炸残留物及环境样品中的NQ、RDX、PETN、CE、HMX、TNT成分。 关键词：炸药，LC, APCI, MS, ASE, GPC, 粉尘 Application of liquid chromatography-atmospheric pressure chemical ionization mass spectrometric in analysis of explosives in powders Xuan Yu1,2，Sun Nan1, Fu De-feng2,Zheng Yi-ping2， Mo Wei-Ming1,Xu Sheng-jie2 1 (College of Chemical Engineering and Materials,Zhejiang University of Technology,Hangzhou 310014) 2（The Forensic Science Institute of Public Security of Zhe Jiang province , Hang Zhou 310009) Abstract: A selective and sensitive LC/APCI-MS/MS was optimized for quantitative analysis of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine(HMX),hexahydro-1,3,5- trinitro-1,3,5-triazine(RDX), pentaerythrite tetranitrate(PETN), tetryl(CE), nitroguanidine(NQ), 2,4,6-trinitrotoluene(TNT) in sandy loam soils. Accelerated solvent extraction (ASE) and Gel Permetion Chromatography(GPC) used as extraction and purification methods,respectively.Sandy loam soils was spiked with explosives,extracted by ASE employed acetone as extraction solvent,purified by GPC used ethyl acetate: cyclohexane (1:1) as mobile phase and the forerun time was 500s, the main faction was 1520s.Instrumental analysis employed 1mmol/L formic acid added to the mobile phase to facilitate formation of formic adduct ions[M+HCOO]-.The method detection limits(MDLs) for HMX, RDX, PETN, CE, NQ and TNT were 0.78，1.44，1.69，0.77，1.06，1.72ng/ml,respectively and recovery were 49.0%~88.4% ,RSD% were 3.5%~10.3%.The method proved effective and was applied to system examination and quantitative analysis of high-ex