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尿样中神经性毒剂代谢产物的HPLC/Q-TOFMS/MS检测方法研究
引用本文:于惠兰,裴承新,胡真,周世坤,赵冲林,王莹.尿样中神经性毒剂代谢产物的HPLC/Q-TOFMS/MS检测方法研究[J].分析测试学报,2010,29(10).
作者姓名:于惠兰  裴承新  胡真  周世坤  赵冲林  王莹
作者单位:防化研究院,北京,102205
摘    要:建立了尿样中甲基膦酸单乙酯(EMPA)、甲基膦酸单异丙酯(IMPA)、甲基膦酸频哪基酯(PMPA)3种神经性毒剂代谢产物的HPLC/Q-TOFMS/MS检测方法。以StrataSi-1型固相萃取小柱对尿样中的3种神经性毒剂代谢产物进行分离,HPLC/Q-TOFESIMS/MS进行测定,内标法定量。该方法对EMPA、IMPA、PMPA的线性范围均为5~320μg/L,相关系数均不低于0.9974;EMPA、IMPA、PMPA的加标回收率分别为57%、98%、81%;检出限(S/N≥3)均为0.1μg/L,定量下限(S/N≥10)均为1μg/L。并将该方法应用于禁化武组织(OPCW)首次生物医学样品分析演练未知尿样的检测,结果满意。

关 键 词:尿样  神经毒剂  代谢产物

Determination of Nerve Agent Metabolites in Urine by High Performance Liquid Chromatography/Quadrupole-Time of Flight Tandem Mass Spectrometry
YU Hui-lan,PEI Cheng-xin,HU Zhen,ZHOU Shi-kun,ZHAO Chong-lin,WANG Ying.Determination of Nerve Agent Metabolites in Urine by High Performance Liquid Chromatography/Quadrupole-Time of Flight Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2010,29(10).
Authors:YU Hui-lan  PEI Cheng-xin  HU Zhen  ZHOU Shi-kun  ZHAO Chong-lin  WANG Ying
Institution:YU Hui-lan,PEI Cheng-xin,HU Zhen,ZHOU Shi-kun,ZHAO Chong-lin,WANG Ying(The Research Institute of Chemical Defense,Beijing 102205,China)
Abstract:A high performance liquid chromatography with quadrupole-time of flight tandem mass spectrometric(HPLC/Q-TOF MS/MS)method was developed for the determination of three nerve agent metabolites,e.g.ethyl methylphosphonic acid(EMPA),isopropyl methylphosphonic acid(IMPA)and pinacolyl methylphosphonic acid(PMPA)in urine.The variable experimental conditions for sample preparation and instruments were optimized.The target compounds were separated on a Strata Si-1 solid phase extraction(SPE)cartridge and analyzed by...
Keywords:HPLC/Q-TOF  MS/MS
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