Dynamic nuclear polarization-enhanced solid-state NMR spectroscopy of GNNQQNY nanocrystals and amyloid fibrils.

Dynamic nuclear polarization-enhanced solid-state NMR spectroscopy of GNNQQNY nanocrystals and amyloid fibrils.
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DOI:
10.1039/c003661g
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发表时间:
2010-06-14
期刊:
Physical chemistry chemical physics : PCCP
影响因子:
--
通讯作者:
Griffin RG
Griffin RG
中科院分区:
其他
文献类型:
--
作者:
Debelouchina GT;Bayro MJ;van der Wel PC;Caporini MA;Barnes AB;Rosay M;Maas WE;Griffin RG

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动态核极化(DNP)利用电子固有的更大极化来增强常规固态NMR实验在低温下的灵敏度。仪器开发和样品制备的最新进展已经改变了这一领域,并为其在生物系统中的应用开辟了新的机会。在这里,我们提出了DNP增强的13 C-13 C和15 N-13 C的相关实验GNNQQNY纳米晶体和淀粉样蛋白原纤维在9.4 T和100 K下获得,并证明DNP可用于获得分配和位点特异性结构信息非常有效。我们研究了温度对这两种体系的分辨率、分子构象、结构完整性和动力学的影响。此外,我们评估了两种常用的固态NMR实验,质子驱动的自旋扩散(PDSD)和转移回波双共振(TEDOR)的低温性能,并讨论了它们作为在低温下结合DNP测量结构相关距离的工具的潜力。
Dynamic nuclear polarization (DNP) utilizes the inherently larger polarization of electrons to enhance the sensitivity of conventional solid-state NMR experiments at low temperature. Recent advances in instrumentation development and sample preparation have transformed this field and have opened up new opportunities for its application to biological systems. Here, we present DNP-enhanced 13C–13C and 15N–13C correlation experiments on GNNQQNY nanocrystals and amyloid fibrils acquired at 9.4 T and 100 K and demonstrate that DNP can be used to obtain assignments and site-specific structural information very efficiently. We investigate the influence of temperature on the resolution, molecular conformation, structural integrity and dynamics in these two systems. In addition, we assess the low-temperature performance of two commonly used solid-state NMR experiments, proton-driven spin diffusion (PDSD) and transferred echo double resonance (TEDOR), and discuss their potential as tools for measurement of structurally relevant distances at low temperature in combination with DNP.
DOI: 10.1016/j.jmr.2009.03.003
发表时间: 2009-06
期刊: Journal of magnetic resonance (San Diego, Calif. : 1997)
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影响因子: 11.1
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