Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by 13C–13C correlation DNP-enhanced NMR

IF 1.8 3区化学 Q4 CHEMISTRY, PHYSICAL

Solid state nuclear magnetic resonance Pub Date : 2023-02-01 DOI:10.1016/j.ssnmr.2022.101850

Adam N. Smith , Rania Harrabi , Thomas Halbritter , Daniel Lee , Fabien Aussenac , Patrick C.A. van der Wel , Sabine Hediger , Snorri Th. Sigurdsson , Gaël De Paëpe

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引用次数: 3

Abstract

We show that multidimensional solid-state NMR ¹³C–¹³C correlation spectra of biomolecular assemblies and microcrystalline organic molecules can be acquired at natural isotopic abundance with only milligram quantities of sample. These experiments combine fast Magic Angle Spinning of the sample, low-power dipolar recoupling, and dynamic nuclear polarization performed with AsymPol biradicals, a recently introduced family of polarizing agents. Such experiments are essential for structural characterization as they provide short- and long-range distance information. This approach is demonstrated on diverse sample types, including polyglutamine fibrils implicated in Huntington's disease and microcrystalline ampicillin, a small antibiotic molecule.

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快速魔角旋转，通过13C–13C相关性DNP增强NMR表征天然同位素丰度下的毫克有机和生物固体

我们表明，生物分子组件和微晶有机分子的多维固态NMR 13C–13C相关光谱可以在天然同位素丰度下仅用毫克量的样品获得。这些实验结合了样品的快速魔角旋转、低功率偶极重新耦合和用最近引入的偏振剂家族AsymPol双自由基进行的动态核偏振。这样的实验对结构表征至关重要，因为它们提供了短距离和长距离的信息。这种方法在不同的样本类型上得到了证明，包括与亨廷顿舞蹈症有关的聚谷氨酰胺原纤维和微晶氨苄青霉素，一种小的抗生素分子。

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来源期刊

Solid state nuclear magnetic resonance 物理-光谱学

CiteScore

5.30

自引率

9.40%

发文量

审稿时长

72 days

期刊介绍： The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.