摘要
三过氧化三丙酮(TATP)的检测分析对于明确爆炸原因,进而对爆炸案件侦破具有重要意义。固相微萃取(SPME)-气质联用法是检测爆炸现场复杂基质中微量TATP的有力手段,已被用于TATP的分析。考虑到商品化SPME涂层众多,有必要系统考察不同涂层的萃取效果,以提升萃取效率。为此,文章系统比较了5种不同SPME涂层对TATP的萃取效果,并优化了SPME萃取条件,包括萃取温度、萃取时间和解吸温度。结果表明,使用PDMS涂层,在萃取温度30℃,萃取时间5 min,解吸温度180℃条件下,萃取效果最佳。该方法在0.1~10μg·mL^(-1)范围内的线性良好(R~2≥0.999),检出限为0.020μg·mL^(-1),比已有方法低一个数量级。6次独立测试结果的相对标准偏差为2.4%,加标回收率为93.2%~101.9%,表明重复性和准确性较好。基于上述方法,成功应用于接触后转移的TATP的检测,为痕量TATP残留物的分析提供了技术参考。
The detection of triacetone triperoxide(TATP) is thus of great significance for clarifying the causes of explosion and detecting the explosion cases.Solid-phase microextraction(SPME)-gas chromatography-mass spectrometry(GC-MS) is a powerful means to detect trace TATP from complex matrix at explosion scenes,and its application for the analysis of TATP has been reported.Given the large number of commercial fibers,it is necessary to systematically investigate different SPME fibers to improve the extraction efficiency.Therefore,the extraction efficiency of five different SPME fibers on TATP was systematically compared,and extraction conditions of SPME were optimized,including extraction temperature and time,as well as desorption temperature.The results indicated that,PDMS fiber exhibited higher extraction efficiency for TATP than the other fibers,and the best extraction efficiency was obtained under the conditions of extraction temperature 30 ℃,extraction time 5 min and desorption temperature 180 ℃.The linear relationship between peak area and concentration of TATP was good enough(R~2≥0.999)from 0.1 μg·mL^(-1) to 10 μg·mL^(-1).The detection limit of TATP was 0.020 μg·mL^(-1),and it is one order of magnitude lower than the existing method.The relative standard deviation of six independent tests was 2.4%,and the spiked recoveries were 93.2%~101.9%,indicating good reproducibility and accuracy.Based on the above method,it has been successfully applied to the detection of TATP transferred after exposure,which provides a technical reference for the analysis of trace TATP residues.
作者
解伟亚
朱军
胡灿
梅宏成
朱晓晗
XIE Wei-ya;ZHU Jun;HU Can;MEI Hong-cheng;ZHU Xiao-han(School of Criminal Investigation,People's Public Security University of China,Beijing 100038,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)
出处
《化学研究与应用》
CAS
北大核心
2024年第1期197-202,共6页
Chemical Research and Application
基金
国家自然科学基金项目(22104018)资助
公安部技术研究计划项目(2020JSYJB08)资助。
关键词
三过氧化三丙酮
顶空固相微萃取
气质联用法
triacetone triperoxide
headspace solid-phase microextraction
gas chromatography-mass spectrometry
