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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
Solid State Nuclear Magnetic Resonance ( IF 1.8 ) Pub Date : 2022-12-20 , DOI: 10.1016/j.ssnmr.2022.101850
Adam N Smith 1 , Rania Harrabi 1 , Thomas Halbritter 2 , Daniel Lee 1 , Fabien Aussenac 3 , Patrick C A van der Wel 4 , Sabine Hediger 1 , Snorri Th Sigurdsson 2 , Gaël De Paëpe 1
Affiliation  

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.



中文翻译:

快速魔角旋转,用于通过 13C-13C 相关 DNP 增强 NMR 表征自然同位素丰度下的毫克量有机和生物固体

我们表明,生物分子组装体和微晶有机分子的多维固态 NMR 13 C- 13 C 相关光谱仅需毫克量的样品即可获得天然同位素丰度。这些实验结合了样品的快速魔角旋转、低功率偶极再耦合和使用 AsymPol 双自由基(最近推出的极化剂家族)进行的动态核极化。此类实验对于结构表征至关重要,因为它们提供了短距离和长距离信息。这种方法在不同的样本类型上得到了证明,包括与亨廷顿氏病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。

更新日期:2022-12-20
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