1D TOCSY技术应用于氨基醇混合物的选择性检测

Selective analysis of the amino alcohols mixtures by 1D TOCSY

对一维全相关谱(1D TOCSY)技术分析高背景干扰下3种痕量氨基醇混合物(三乙醇胺、N-甲基二乙醇胺、2-二异丙基氨基乙醇)进行了研究。优化了脉冲序列、整形脉冲、混合时间等关键实验参数,实现对3种痕量氨基醇化合物相关峰的指认和结构鉴定,方法检测限为5μg/mL。在三乙醇胺的氢谱信号完全被掩盖或干扰的情况下,讨论了利用1D TOCSY定量分析三乙醇胺的可行性。将建立的1D TOCSY方法成功应用于国际禁止化学武器组织(OPCW)第42次水平考试的盲样分析。与1D NOESY方法相比,1D TOCSY方法在实现选择性检测的同时,具有更高的检测灵敏度,有利于痕量分析。

1D TOCSY was applied to detect and identify the mixture of three amino alcohols (triethanolamine,methyldiethanolamine and 2-(diisopropylamino)ethanol)at trace level with high background..The key experimental parameters,such as pulse sequence,shaped pulse and mixing time were optimized.The LODs of this method for these three chemicals were 5μg/mL.In the case that the 1H-NMR signals of triethanolmnine are completely covered or interfered,the feasibility of using 1D TOCSY for quantitative analysis is discussed.The established 1D TOCSY method was applied to the analysis of the blind sample in the 42th OPCW proficiency test.Compared with 1D NOESY,1D TOCSY can not only realize the purpose of selective analysis of the mixtures but also is more helpful in trace analysis with higher sensitivity.