提出了高效液相色谱-串联质谱法(HPLC-MS/MS)测定爆炸尘土中梯恩梯(TNT)、特屈儿(CE)、太安(PETN)、奥克托金(HMX)、黑索今(RDX)等5种常见有机炸药含量的方法。称取爆炸尘土10 g,加入20 mL丙酮,混匀,离心,取上清液,用氮气吹干,再加入1 mL甲醇,超声溶解,用0.22 μm有机滤膜过滤。以不同体积比的0.5 mmol·L^-1乙酸铵溶液-甲醇为流动相进行梯度洗脱。质谱分析中采用电喷雾离子源负离子(ESI^-)模式和多反应监测(MRM)模式进行检测。结果显示:5种有机炸药的质量分数在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)为0.033~0.05 μg·kg^-1;对空白尘土样品进行3个浓度水平的加标回收试验,回收率为61.6%~99.0%,日内精密度(n=5)为1.1%~7.1%,日间精密度(n=5)为4.2%~9.8%。方法用于实际样品分析,TNT的检出量为67.7 μg·kg^-1,其余4种有机炸药未检出。

A method for the determination of 5 organic explosives, including of trinitrotoluene (TNT), 2,4,6-trinitrobenzylamine (CE), pentaerythritol tetranitrate (PETN), cyclotetramethylene tranitramine (HMX), cyclotrimethylene trinitramine (RDX), in explosion dust by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was proposed. 10 g of explosive dust was added into 20 mL of acetone. After mixing well and centrifugation, the supernatant was blew to dry with nitrogen. Then 1 mL of methanol was added, and the above solution was dissolved by ultrasound and filtered with 0.22 μm organic filter membrane. A mixture of 0.5 mmol·L^-1 ammonium acetate solution and methanol at different volume ratios was used as mobile phase for gradient elution. ESI^- mode and MRM mode were used for MS analysis. As shown by the results, linear relationships between values of mass fraction of 5 organic explosives and their peak areas were kept in definite ranges, with detection limits (3S/N) in the range of 0.033-0.05 μg·kg^-1. Test for recovery was made on the blank dust sample at 3 concentration levels by standard addition method, giving results in the range of 61.6%-99.0%, and intra-day precision (n=5) and inter-day precision (n=5) were in the ranges of 1.1%-7.1% and 4.2%-9.8%. This method has been applied to the analysis of actual samples, giving detection amount of 67.7 μg·kg^-1 for TNT, and the other 4 organic explosives were not detected.