气相色谱-三重四极杆串联质谱检测尿样中神经性毒剂代谢产物烷基膦酸类化合物
发布日期：2019-08-13 来源：分析测试学报 浏览数：1729 人
作者
杨旸，闫珑 ，李晓森，袁铃，邢中方，刘石磊
单位
1.军事科学院防化研究院分析测试中心；2.国民核生化灾害防护国家重点实验室
中文摘要:建立了气相色谱-三重四极杆串联质谱检测尿样中有机磷毒剂代谢产物烷基膦酸类化合物含量的方法。选用DB-17MS色谱柱(30 m×0.25 mm×0.25 μm)，化学离子源，在负离子模式下，选择反应监测模式扫描，对暴露于有机磷毒剂下的人尿样中的烷基膦酸类化合物含量进行测定。在优化条件下，5种烷基膦酸类化合物可在30 min内完成同时测定，检测方法的线性关系良好，检出限为0.1 μg/L，定量下限为0.5 μg/L，加标回收率为97.3%~98.9%，重复性RSD为5.3%~10%，日内相对标准偏差(RSD)为2.4%~4.3%，日间RSD为2.5%~4.5%。该法准确、灵敏度高、专属性强、重复性好，适用于染毒尿样中烷基膦酸类化合物的含量测定，可为有机磷毒剂人体内代谢产物烷基膦酸类化合物提供有效的检测手段。
中文关键词:气相色谱-串联质谱(GC-MS/MS) 烷基膦酸类化合物 氟化衍生 体外染毒尿样
Determination of Alkyl Phosphoric Acids，Metabolites of Nerve Agents in Urine by Gas Chromatography-Triple Quadrupole Mass Spectrometry
Abstract:A gas chromatography-triple quadrupole mass spectrometric(GC-MS/MS) method was established for the determination of alkyl phosphoric acids，metabolites of organophosphorus nerve agents in urine.The samples exposed to organophosphorus nerve agents were detected by MS/MS using chemical ion source(CI ) in negative ion mode under selected reaction monitoring(SRM) mode.Both quantification and confirmation ions were optimized for each of 5 alkyl phosphoric acids.5 alkyl phosphoric acids were simultaneously detected in 30 min.The calibration curves for the analytes were linear in the certain concentration ranges with the limits of detection(LOD) and quantitation(LOQ) of 0.1 μg/L and 0.5 μg/L，respectively.The intra-day and inter-day RSDs were in the range of 2.4%-4.3% and 2.5%-4.5%，respectively.The average recoveries were in the range of 97.3%-98.9% and the RSDs for the method repeatability were 5.3%-10%.With the advantages of excellent selectivity，accuracy，high sensitivity，specificity and good repeatability，the method is suitable for the qualitative and quantitative detections of alkyl phosphoric acids in urine samples exposed to organophosphorus nerve agents.
Key Words:gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS) alkyl phosphoric acids fluorinated derivatization urine exposed to organophosphorus nerve agents
引用本文：杨旸，闫珑 ，李晓森，袁铃，邢中方，刘石磊.气相色谱-三重四极杆串联质谱检测尿样中神经性毒剂代谢产物烷基膦酸类化合物[J].分析测试学报,2018,37(9):1082-1086.
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