Single-Scan Multidimensional NMR Analysis of Mixtures at Sub-Millimolar Concentrations by using SABRE Hyperpolarization
Single-Scan Multidimensional NMR Analysis of Mixtures at Sub-Millimolar Concentrations by using SABRE Hyperpolarization
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DOI：
10.1002/cphc.201500535
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发表时间：
2015-11-16
期刊：
影响因子：
2.9
通讯作者：
Huber, Gaspard
中科院分区：
文献类型：
--
作者：
Daniele, Valeria;Legrand, Francois-Xavier;Huber, Gaspard
可逆交换信号放大（SABRE）是一种提高核磁共振（NMR）实验灵敏度的有效方法。然而，SABRE增强的H-1 NMR信号是短暂的，并且SABRE通常仅用于记录1D NMR谱。当感兴趣的样品是复杂的混合物时，这导致H-1光谱的严重重叠。此外，使用共底物，其信号可能会掩盖H-1光谱，是目前降低SABRE实验检测限的最有效方法。在这里，我们描述了一种方法来获得清洁，SABRE-hyperpolarized二维H-1 NMR光谱的混合物的小分子在亚毫摩尔浓度在一个单一的扫描。该方法依赖于使用仲氢与氘代共底物一起用于超极化和超快2D NMR用于采集。它适用于所有可以用SABRE偏振的基板。
Signal amplification by reversible exchange (SABRE) is a promising method to increase the sensitivity of nuclear magnetic resonance (NMR) experiments. However, SABRE-enhanced H-1 NMR signals are short lived, and SABRE is often used to record 1D NMR spectra only. When the sample of interest is a complex mixture, this results in severe overlaps for H-1 spectra. In addition, the use of a co-substrate, whose signals may obscure the H-1 spectra, is currently the most efficient way to lower the detection limit of SABRE experiments. Here, we describe an approach to obtain clean, SABRE-hyperpolarized 2D H-1 NMR spectra of mixtures of small molecules at sub-millimolar concentrations in a single scan. The method relies on the use of para-hydrogen together with a deuterated co-substrate for hyperpolarization and ultrafast 2D NMR for acquisition. It is applicable to all substrates that can be polarized with SABRE.