Pure Shift Proton NMR: A Resolution of the Resolution Problem?

纯位移质子核磁共振：解决分辨率问题？

• 批准号: EP/I007989/1
• 负责人: Gareth Morris
• 金额: $ 61.47万
• 依托单位: University of Manchester
• 依托单位国家: 英国
• 项目类别: Research Grant
• 财政年份: 2010
• 资助国家: 英国
• 起止时间: 2010 至 无数据
• 项目状态: 已结题
• 来源: https://gtr.ukri.org/projects?ref=EP%2FI007989%2F1
• 关键词: Pure; Shift; Proton; NMR; Resolution

Proton (hydrogen) nuclear magnetic resonance (NMR) spectroscopy is the single tool most widely used by chemists for determining the molecular structures of unknown compounds. It is a wonderfully versatile and sensitive tool, but it has a major drawback: it struggles to separate the signals from the different hydrogen atoms in a molecule, because each atom typically gives rise to multiple signals. This multiplicity of signals arises because of the magnetic interactions between hydrogen nuclei, and it typically leads to spectra being about ten times more crowded than would be the case if these interactions could be switched off. Unfortunately, while such a broadband decoupling is routine where interactions between different types of atom (e.g. hydrogen and carbon) are involved, there is no general way of achieving it for interactions between atoms of the same type. What we have recently shown, however, is that by suitable choice of experimental methods we can in many cases reverse the effects of interactions, allowing us to measure pure shift spectra in which a single signal is seen for each hydrogen atom in a molecule. The simplicity such techniques offer means that we should be able to resolve the signals of individual atoms in much larger species, or in much more complex mixtures, than is currently the case. At the moment the only way to resolve signals better is to spread them out by using a higher magnetic field, but progress in building better magnets is agonisingly slow - over the last 30 years the highest field available has increased on average by just a few per cent each year. With pure shift methods we should be able to get almost a tenfold improvement in the space of a few years. In this project, a postdoctoral research fellow and a postgraduate student will investigate turning our initial proof of principle into practical tools. If they are successful, these tools will end up being used by chemists, biochemists and other scientists all over the world.

质子（氢）核磁共振（NMR）光谱是化学家最广泛使用的确定未知化合物分子结构的单一工具。它是一种非常通用和敏感的工具，但它有一个主要的缺点：它很难将信号从分子中的不同氢原子中分离出来，因为每个原子通常会产生多个信号。这种信号的多样性是由于氢原子核之间的磁相互作用而产生的，它通常会导致光谱比如果这些相互作用可以被关闭的情况拥挤大约十倍。不幸的是，虽然这种宽带去耦在涉及不同类型的原子（例如氢和碳）之间的相互作用的情况下是常规的，但是对于相同类型的原子之间的相互作用，没有通用的方法来实现它。然而，我们最近发现，通过适当选择实验方法，我们可以在许多情况下逆转相互作用的影响，使我们能够测量纯位移光谱，其中分子中的每个氢原子都可以看到单一信号。这种技术提供的简单性意味着我们应该能够在比目前更大的物种或更复杂的混合物中解析单个原子的信号。目前，更好地解析信号的唯一方法是通过使用更高的磁场来分散信号，但制造更好的磁铁的进展非常缓慢-在过去的30年里，最高的磁场平均每年只增加几个百分点。使用纯移位法，我们应该能够在几年的时间内得到几乎十倍的改进。在这个项目中，一名博士后研究员和一名研究生将研究如何将我们最初的原理证明转化为实用工具。如果他们成功了，这些工具最终将被全世界的化学家、生物化学家和其他科学家使用。

项目成果

Ultra-high dispersion NMR reveals new levels of detail

超高色散核磁共振揭示了新的细节水平

• DOI: 10.1039/c5ra10192a
• 发表时间: 2015
• 期刊: RSC Advances
• 影响因子: 3.9
• 作者: Aguilar J

Systematic comparison of sets of (13)C NMR spectra that are potentially identical. Confirmation of the configuration of a cuticular hydrocarbon from the cane beetle Antitrogus parvulus.

• DOI: 10.1021/jo5012027
• 发表时间: 2014-08-15
• 期刊: The Journal of organic chemistry
• 作者: Basar N;Damodaran K;Liu H;Morris GA;Sirat HM;Thomas EJ;Curran DP
• 通讯作者: Curran DP

Decoupling Two-Dimensional NMR Spectroscopy in Both Dimensions: Pure Shift NOESY and COSY

• DOI: 10.1002/anie.201108888
• 发表时间: 2012-01-01
• 期刊: ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
• 影响因子: 16.6
• 作者: Aguilar, Juan A.;Colbourne, Adam A.;Morris, Gareth A.
• 通讯作者: Morris, Gareth A.