液相色谱电喷雾飞行时间质谱检测泥土中神经性毒剂降解产物  

Determination of Degradation Products of Nerve Agents in Soil by Liquid Chromatography-Time of Flight-Mass Spectrometry with Electrospray Ionization

作　　者：刘勤[1] 胡绪英[1] 谢剑炜[1] 

机构地区：[1]军事医学科学院毒物药物研究所,北京100850

出　　处：《分析化学》2004年第10期1309-1313,共5页Chinese Journal of Analytical Chemistry

摘　　要：采用液相色谱 电喷雾飞行时间质谱对 6种神经性毒剂的降解产物烷基甲基膦酸同时进行定性、定量检测。对经过液相色谱分离后的化合物进行源内碰撞诱导裂解 (CID) ,并对化合物及其碎片离子进行精确质量测定 ,测定质量与理论质量之间误差不超过 2 .5mDa。采用优化后的实验条件及选择离子检测法对化合物进行定量分析 ,给出了 6种烷基甲基膦酸的线性范围和回归曲线 ,检出限为 0 .2 5～ 5ng ;RSD均小于8 8%。将本法用于染毒泥土样品的检测 ,表明该法简便、快速、准确。For proof of the presence of chemical nerve agents, a rap id, accurate and sensitive method which a allowed used to determine their degradation products alkyl methylphosphonic acids was developed by using liquid chromatography-time of flight-mass spectrometry with electrospray ionization., With in-source collision induced dissociation (CID) and exact mass measurement, the differences between the calculated mass and the theoretical mass of all compounds and fragments were less than 2.5 mDa. Quantitative measurement was performed by mass spectrometry in selected ion monitoring mode with chromatographic separation. Linear calibration curves were obtained for the six kinds of alkyl methylphosphonic acids, and the detection limits were 0.25 similar to 5 ng. The RSD was less than 8.8 %. The method has also been applied to detect the contaminated soil samples and was proved to be simple, rapid and accurate.

关 键 词：液相色谱 电喷雾飞行时间质谱 泥土 神经性毒剂 降解产物 源内碰撞诱导裂解 精确质量测定 化学战剂 土壤污染化学 

分 类 号：O657.63[理学—分析化学]