Abstract:

Objective To establish an LC-ESI-MS/MS method for the determination of glyceryl trinitrate（NG） in soil samples and to make basis for the detection of explosive residues of NG. Method The liquid-liquid extraction method was adopted to extract analytes. The extraction solvents and mobile phase were optimized. The influence of mass parameter was also examined. Results Methanol was used as the extraction solvent. The separation was performed on an SB C18 column（4.6×150mm， 5μm）. High sensitivity was achieved with 0.05mmol/L of ammonium chloride in methanol used as the mobile phase. The limit of detection was 0.25ng/g for NG in the standard solution. High recovery（90.4%～95.2%） was achieved. Good linearity （R2>0.9990） was obtained at low concentrations （0.25～10ng/g）. Conclusion This method is simple， accurate and sensitive and can be used in trace NG detection for explosive residues.

Key words: LC-ESI-MS/MS, soil sample, glyceryl trinitrate, additive

摘要：

目的 建立了高效液相色谱-质谱/质谱法（LC-ESI-MS/MS）测定尘土中的硝化甘油（NG）的方法，为日后测定爆炸残留物中的NG奠定基础。方法 采用液液提取的方式提取样品，考察了前处理条件、色谱条件及质谱参数，最终确定实验方法。结果 选择了最佳液相色谱质谱分析方法：固定相为SB C18（4.6×150 mm，5 μm），甲醇—0.05 mmol氯化铵做流动相，甲醇作提取溶剂；该方法在0.25～10 ng/g范围内呈良好线性，相关系数为0.9990；定量下限为0.25 ng/g；加标回收率为90.4%～95.2%。结论 本方法操作简单，提取方便，有效避免了尘土复杂基质的干扰，结果准确可靠，灵敏度高，满足对爆炸残留物中硝化甘油的检测要求。

关键词: 液相色谱-电喷雾串联质谱, 尘土, 硝化甘油, 添加剂