环境样品中痕量硫芥类化合物的核磁共振分析  

Nuclear magnetic resonance analysis of trace sulfur mustard chemicals in the environmental samples

作　　者：王栋 夏俊美 张盈盈 吕家乐 袁铃 黄桂兰 WANG Dong;XIA Junmei;ZHANG Yingying;LV Jiale;YUAN Ling;HUANG Guilan(State Key Laboratory of NBC Protection for Civilian,Beijing 102205,China;School of Chemistry and Chemical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China;School of Chemical Engineering,Sichuan University of Science&Engineering,Zigong 643002,China)

机构地区：[1]国民核生化灾害防护国家重点实验室,北京102205 [2]南京理工大学化学与化工学院,南京210094 [3]四川轻化工大学化学工程学院,自贡643002

出　　处：《分析试验室》2023年第5期689-695,共7页Chinese Journal of Analysis Laboratory

摘　　要：采用核磁共振(NMR)技术对有机废液和废水样品中的痕量硫芥类化合物进行了筛查和鉴定分析。通过氢谱(1H-NMR)比对策略和一维全相关谱(1D TOCSY)技术对原样进行无损筛查分析。将1D TOCSY-TOCSY双选择性激发技术和一维化学位移选择性滤波-全相关谱(1D CSSF-TOCSY)应用于筛查未知样品中所含的硫芥类化合物。为满足1H-NMR谱图鉴定标准,采用液液萃取、溶剂置换、固相萃取等样品前处理技术消除了目标化合物信号的干扰。通过1H-NMR谱图比对的方式,提供了芥子气、 1,3-双(乙烯基硫醚)丙烷和1, 3-双(2-羟基乙基砜)丙烷3个化合物的鉴定证据。本文所采用的分析策略和方法,可为禁止化学武器公约组织化武履约核查样品中痕量化武相关化合物的1H-NMR分析鉴定提供参考。Nuclear magnetic resonance(NMR)technique was used to screen and identify trace sulfur mustard chemicals in the organic and aqueous waste samples.1H-NMR and one dimensional total correlation spectroscopy(1D TOCSY)were used for non-destructive screening analysis of the original samples.1D TOCSY-TOCSY and 1D TOCSY incorporated with a chemical shift selective filter(1D CSSF-TOCSY)were applied in screening the contained sulfur mustard related compounds in the unknown samples.In order to meet the criteria for 1H-NMR data presentation,sample pretreatment technologies including liquid-liquid extraction,solvent exchange and solid phase extraction were used to eliminate the interference of the target resonances.Bis(2-chloroethyl)sulfide,1,3-Bis(vinylthio)propane and 1,3-Bis(2-hydroxyethylsulfonyl)propane were identified based on 1HNMR spectra comparison.The results were in good agreement with the list of spiking chemicals.The analytical strategies of this work can provide reference for the 1H-NMR analysis of the trace chemical warfare related compounds in official OPCW proficiency test.

关 键 词：硫芥类化合物 核磁共振 化武核查 痕量分析 一维全相关谱 

分 类 号：O657.61[理学—分析化学]