采用高选择性和灵敏度的LC(液相色谱)/APCI(大气压化学电离源)/MS(质谱)方法定量分析粉尘样品中的HMX、RDX、PETN、CE、NQ和TNT.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,用丙酮作为ASE萃取溶剂,乙酸乙酯和环己烷(体积比为1∶1)作为GPC净化时的流动相并抛弃杂质500s,收集1 520 s.在LC/MS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.结果表明,HMX、RDX、PETN、CE、NQ、TNT的方法检测限分别为0.78,1.44,1.69,0.77,1.06,1.72 ng/mL,回收率为49.0％～88.4％,相对标准偏差为3.5％～10.3％.该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.%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-l, 3 , 5-triazine (RDX), pentaerythrite tetranitrate (PETN), tetryl(CE), nitroguanidine(NQ), 2 ,4, 6-trinitrotolueneCTNT) in sandy loam soils. Accelerated solvent extraction (ASE) and Gel permetion chromatography(GPC) were used as extraction and purification methods, re spectively. 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. The LC/MS analysis employed lmmol/L formic acid added to the mobile phase to facilitate for mation 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 could be applied in the system examination and quantitative analysis of high-explosives in exploded residues and environmental samples.
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