HPLC-MS/MS检测爆炸尘土中的二硝基重氮酚  

Detection of Diazodinitrophenol in Post-blast Dust by HPLC-MS/MS

作　　者：王文豪[1,2] 张榆梓 周红[4] 孙玉友[4] 梅宏成[4] 刘占芳[4] 陈涛[2,4] 马捷[5] 仲利静[4] 

机构地区：[1]石家庄市栾城区国家税务局,石家庄051430 [2]中国人民公安大学刑事科学技术学院,北京100038 [3]内蒙古自治区公安厅,呼和浩特010051 [4]公安部物证鉴定中心,北京100038 [5]石家庄市公安局桥西分局,石家庄050000

出　　处：《刑事技术》2016年第2期107-110,共4页Forensic Science and Technology

基　　金：国家十二五科技支撑计划课题(No.2012BAK02B04)

摘　　要：目的建立爆炸尘土中二硝基重氮酚的高效液相色谱-串联质谱（HPLC-MS/MS）检测方法,解决实际案例中二硝基重氮酚难以检测的问题。方法爆炸尘土用丙酮浸提,经离心后取上清液,浓缩定容。用Agilent XDB-C18色谱柱（150 mm×4.6 mm,5μm）分离,用甲醇和水（70：30,V/V）作为流动相,等度洗脱,电喷雾离子源（ESI）在多反应监测模式（MRM）下进行负离子扫描,使用外标法定量。结果二硝基重氮酚在0.5~200.0 ng/m L范围内质量浓度与峰面积线性关系良好,相关系数r2=0.9994。方法检出限（S/N=3）和定量限（S/N=10）分别为0.04 ng/g和0.12 ng/g。以空白尘土为基体,在添加浓度为0.2、10.0、40.0 ng/g时进行回收率实验,平均回收率在87.0%~95.1%之间,日内、日间精密度分别在2.58%~3.97%与4.17%~6.23%之间。进行二硝基重氮酚爆炸验证试验,在实际爆炸尘土中均检出二硝基重氮酚。结论本文所建方法简便、快速、灵敏度高,适用于对爆炸尘土中二硝基重氮酚的检测,解决了实际案件中二硝基重氮酚难以检测的迫切问题。Objective To develop a method for detection of diazodinitrophenol（DDNP） in post-blast dust based on high performance liquid chromatography-tandem mass spectrometry. Methods The post-blast dust was extracted by acetone, then centrifugated to get supernatant. The volume of supernatant fluid was concentrated and readjusted by methanol. The separation was performed on an Agilent XDB-C18 column（150 mm×4.6 mm, 5 μm） with isocratic elution of methanol and water（70：30,V/V）. MS/MS was adopted in the multi-reactions monitoring mode via negative electro-spray ionization setup. Results Linear relationship was kept between peak area and DDNP mass concentration in the range of 0.5~200 ng/m L（r2=0.9994）, with detection limit（S/N=3） of 0.04 ng/g and quantization limit（S/N=10） of 0.12 ng/g. The average recoveries spiked at 3 levels of 0.2, 10.0 and 40.0 ng/g were in the range of 87.0 %~95.1 %, with intra- and inter-day precision of 2.58 %~3.97 % and 4.17 %~6.23 %, respectively. An explosive verification experiment for DDNP was conducted and successfully detected the substance in the post-blast dust. Conclusions This method is convenient, rapid and sensitive, suitable for detection of DDNP in post-blast dust, bringing forth a solution for the urgency difficult to detect DDNP in real cases.

关 键 词：起爆药 爆炸残留物 液相色谱-串联质谱 二硝基重氮酚 雷管 爆炸尘土 

分 类 号：DF794.3[政治法律—诉讼法学]