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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 establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of dinitro diazo-phenols in explosive dust and to solve the problem that dinitro diazo phenols are difficult to detect in practical cases. Methods Explosion dust was extracted with acetone, the supernatant was centrifuged and concentrated to volume. Separation was performed on an Agilent XDB-C18 column (150 mm × 4.6 mm, 5 μm) eluting isocratically using methanol and water (70:30, V / V) as the mobile phase. Electrospray ionization (ESI) Negative ion scan under monitoring mode (MRM), quantified using external standard. Results The linear relationship between mass concentration and peak area of dinitrotrehydrophenol in the range of 0.5 ~ 200.0 ng / m L was good. The correlation coefficient r2 was 0.9994. The limits of detection (S / N = 3) and the limit of quantitation (S / N = 10) were 0.04 ng / g and 0.12 ng / g, respectively. The recovery rate was tested with blank dust as substrate. The average recoveries were between 87.0% and 95.1% at the concentrations of 0.2, 10.0 and 40.0 ng / g. The intra-day and inter-day precision were between 2.58% and 3.97% 4.17% ~ 6.23% between. Dinitro diazo phenol explode verification test, dinitro diazo phenols were detected in the actual explosion dust. Conclusion The method proposed in this paper is simple, rapid and sensitive. It is suitable for the detection of dinitro diazo phenols in explosive dust and solves the urgent problem that it is difficult to detect dinitro diazo phenols in practical cases.