一维NOESY技术在醇胺混合物分析中的应用

Analysis of the alcohol amine mixtures by 1D selective NOESY

N-甲基二乙醇胺、三乙醇胺、2-二异丙基氨基乙醇分别属于化武相关化合物氮芥气HN2、氮芥气HN3、神经性毒剂Vx前体化合物。采用一维NOESY选择性激发核磁共振技术实现了高背景干扰下对痕量3种醇胺类化合物相关峰的指认和结构的鉴定。方法对三乙醇胺、N-甲基二乙醇胺、2-二异丙基氨基乙醇检测限(S/N>3)分别为5,10,10μg/m L。该方法简单、快速、不需要复杂的样品前处理步骤,可以有效排除背景干扰,解决核磁共振氢谱中目标化合物部分峰被掩盖,无法对化合物实施充分鉴定的情况。以第32次禁化武组织的水平考试编号322的有机样品为基质,添加20μg/m L 3种醇胺化合物,使用该方法进行分析,取得了良好的效果。

N-methyldiethanolamine, tris （2-hydroxyethyl） amine, 2 - （diisopropylamino） ethanol are the precursors of nitrogen mustard HN2, nitrogen mustard HN3, nerve agent Vx respectively. 1D selective NOESY method was usedsuccessfullyto detect and identify three alcohol amines at trace level with high background. The LODs of this method for the determination of tris （2-hydroxyethyl） amine, N-methyldiethanolamine, 2- （diisopropylamino）ethanol was 5, 10 and 10 μg/mL respectively. This method was simple, fast and can wipe off the interference effectively in thelH NMR spectrum without complex sample pretreatment. It was useful for the identification of the target chemicals when their peaks were partly covered in 1H NMR spectrum. These three chemicals at 20 μg/mL were spiked in the organic samplewhich code number was 322 from 32th OPCW Official Proficiency Tests and were analyzed successfully with this method.