通过一维 TOCSY 技术定性分析芳香族化合物

Wenbo Dong , Qi Zhao , Jiancheng Zhao , Jiarong Zhang , Yingxiong Wang , Yan Qiao
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引用次数: 0

摘要

芳香族化合物包括邻二甲苯、间二甲苯、对二甲苯和乙苯,主要来源于原油的催化重整,用途广泛。然而,由于物理和化学性质相似,这些化合物在没有标准样品的情况下很难通过气相色谱法(GC)进行鉴别。随着现代核磁共振(NMR)技术的发展,NMR 已成为无需纯化即可快速分析复杂粗混合物的强大而高效的工具。本研究优化了一维(1D)全相关光谱(TOCSY)核磁共振技术的参数,包括一维选择性梯度 TOCSY 和一维化学位移选择性过滤(CSSF)与 TOCSY,以获得全面的分子结构信息。结果表明,非极性芳香族化合物(包括邻二甲苯、间二甲苯、对二甲苯和乙苯)、极性芳香族化合物(苯甲醇、苯甲醛、苯甲酸)以及带有额外共轭键的芳香族化合物(苯乙烯)的核磁共振光谱中的重叠信号都能在一维 TOCSY 中得到解析。更重要的是,通过在一维 TOCSY 中设置适当的混合时间,可以清晰地分辨出完整的分子结构。这种方法简化了 NMR 图谱,提供了整个分子的结构信息,并可用于分析其他结构异构体。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Qualitative analysis of aromatic compounds via 1D TOCSY techniques

Qualitative analysis of aromatic compounds via 1D TOCSY techniques

The aromatic compounds, including o-xylene, m-xylene, p-xylene, and ethylbenzene, primarily originate from the catalytic reforming of crude oil, and have a wide variety of applications. However, because of similar physical and chemical properties, these compounds are difficult to be identified by gas chromatography (GC) without standard samples. With the development of modern nuclear magnetic resonance (NMR) techniques, NMR has emerged as a powerful and efficient tool for the rapid analysis of complex and crude mixtures without purification. In this study, the parameters of one-dimensional (1D) total correlation spectroscopy (TOCSY) NMR techniques, including 1D selective gradient TOCSY and 1D chemical-shift-selective filtration (CSSF) with TOCSY, were optimized to obtain comprehensive molecular structure information. The results indicate that the overlapped signals in NMR spectra of nonpolar aromatic compounds (including o-xylene, m-xylene, p-xylene and ethylbenzene), polar aromatic compounds (benzyl alcohol, benzaldehyde, benzoic acid), and aromatic compounds with additional conjugated bonds (styrene) can be resolved in 1D TOCSY. More importantly, full molecular structures can be clearly distinguished by setting appropriate mixing time in 1D TOCSY. This approach simplifies the NMR spectra, provides structural information of entire molecules, and can be applied for the analysis of other structural isomers.

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来源期刊
Magnetic Resonance Letters
Magnetic Resonance Letters Analytical Chemistry, Spectroscopy, Radiology and Imaging, Biochemistry, Genetics and Molecular Biology (General)
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