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实时二维核磁共振对连续色谱分离过程中分析物的鉴定。

Real-time 2D NMR identification of analytes undergoing continuous chromatographic separation.

作者信息

Shapira Boaz, Karton Amir, Aronzon Dina, Frydman Lucio

机构信息

Department of Chemical Physics, Weizmann Institute of Science, 76100 Rehovot, Israel.

出版信息

J Am Chem Soc. 2004 Feb 4;126(4):1262-5. doi: 10.1021/ja0389422.

DOI:10.1021/ja0389422
PMID:14746499
Abstract

We have recently proposed and demonstrated an approach that enables the acquisition of multidimensional nuclear magnetic resonance (NMR) spectra within a single scan. A promising application opened up by this new accelerated form of data acquisition concerns the possibility of monitoring in real time the chemical nature of analytes subject to a continuous flow. The present paper illustrates such potential, with the real-time acquisition of a series of 2D 1H NMR spectra arising from a mixture of compounds subject to a continuous liquid chromatography (LC) separation. This real-time 2D NMR identification of chemicals eluted minutes apart under usual LC-NMR conditions differs from the way in which LC-2D NMR has hitherto been carried out, which relies on stopped-flow modes of operations whereby fractions are first collected and then subject to individual, aliquot-by-aliquot analyses. The real-time LC-2D NMR experiment hereby introduced can be implemented in a straightforward manner using modern commercial LC-NMR hardware, thus opening up immediate possibilities in high-throughput characterizations of complex molecules.

摘要

我们最近提出并证明了一种方法,该方法能够在单次扫描中获取多维核磁共振(NMR)光谱。这种新的加速数据采集形式开辟了一个有前景的应用领域,即有可能实时监测连续流动的分析物的化学性质。本文阐述了这种潜力,通过实时采集一系列二维¹H NMR光谱,这些光谱来自经过连续液相色谱(LC)分离的化合物混合物。在通常的LC-NMR条件下,对相隔几分钟洗脱的化学物质进行实时二维NMR鉴定,这与迄今为止进行LC-2D NMR的方式不同,后者依赖于停流操作模式,即首先收集馏分,然后对每个馏分进行逐份分析。本文介绍的实时LC-2D NMR实验可以使用现代商用LC-NMR硬件以直接的方式实现,从而为复杂分子的高通量表征开辟了直接的可能性。

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引用本文的文献

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