Multifrequency microwave powered DNP instrument for MAS NMR

用于 MAS NMR 的多频微波供电 DNP 仪器

• 批准号: 9166814
• 负责人: Songi Han
• 金额: $ 19.98万
• 依托单位: UNIVERSITY OF CALIFORNIA SANTA BARBARA
• 依托单位国家: 美国
• 财政年份: 2016
• 资助国家: 美国
• 起止时间: 2016-08-01 至 2018-05-31
• 项目状态: 已结题
• 来源: https://reporter.nih.gov/project-details/9166814
• 关键词: Address; Alzheimer' s Disease; Amyloid Fibrils; Attention; Automobile Driving; Biological; Cells; Characteristics; Collaborations; Detection; Development; Device or Instrument Development; Devices; Diagnostic; Electron Spin Resonance Spectroscopy; Event; Freezing; Frequencies; Funding; Generations; Hand; Helium; Home environment; Label; Laboratories; Liquid substance; Magic; Measurement; Membrane Proteins; Methods; Modification; NMR Spectroscopy; Nitrogen; Nuclear; Optics; Pattern; Peptides; Performance; Physiologic pulse; Power Sources; Proteins; Pump; Research; Research Design; Research Infrastructure; Resolution; Role; Sampling; Signal Transduction; Solid; Solvents; Source; Staging; Structure; System; Techniques; Technology; Temperature; Testing; Time; base; cost; design; improved; innovation; instrument; instrumentation; irradiation; magnetic field; microwave electromagnetic radiation; novel; operation; protein aggregate; protein aggregation; research study; solid state; stem; structural biology; success; tool; transmission process

PROJECT SUMMARY Solid-state dynamic nuclear polarization (ssDNP) is an NMR signal-enhancing technique by on-resonant microwave (MW) irradiation of tailored radical-based DNP agents that is attracting dramatic attention in recent years, given its potential to transform the capability of NMR spectroscopy for structural biology as we know it, in particular of solid-state magic angle spinning (MAS) NMR studies of biological solid samples. The potential of ssDNP stems from the ability of this technique to enhance spin polarization by O(102-103) fold. This signal gain, combined with a thermal polarization gain of O(101) fold from cooling to liquid nitrogen temperatures and O(102) from cooling to liquid helium temperatures, together with high magnetic fields, offers a total signal gain of up to O(105) for ssNMR, and accordingly a reduction in experimental time by up to the square of this signal gain. Such dramatic magnitudes of signal enhancement enable unprecedented ssNMR studies of the types of samples and conditions that have been inaccessible to NMR based structure studies before. Among the ssDNP-enabled research highlights are the study of membrane protein systems in whole cells or the study of inter-strand structure determination of the quaternary structure of amyloid fibrils. A particular focus of our development is to enable transient structure studies of aggregating proteins by ssDNP-enhanced MAS NMR of freeze-quenched proteins at various stages of aggregation. In the well-recognized role of ssDNP to enhance MAS NMR as an ultimate high- resolution structural biology tool to capture transiently evolving structures, we propose to address major technological challenges with our innovative instrument developments. The core of our development will be a compact and versatile quasi-optical MW bridge design with novel two-frequency pump, concurrent DNP and EPR, as well as ELDOR capabilities under MAS operation. While, ssDNP-enhanced MAS NMR is the center of focus of contemporary NMR as it has the potential to transform MAS NMR structure studies of biosolids, only a handful of alternative ssDNP MAS NMR instruments exists in the world to the commercial gyrotron-powered ssDNP MAS NMR instrument operating at >100 Kelvin—our instrumental platform for DNP-enhanced MAS NMR aims to offer an alternative solution with greater versatility and performance.

项目摘要 固态动力学核极化（SSDNP）是一种NMR信号增强技术（MW） 近年来引起极大的关注的量身定制的基于自由基的DNP剂的辐照，鉴于其潜力 正如我们所知，转化NMR光谱对结构生物学的能力，尤其是固态魔法角度 生物固体样品的旋转（MAS）NMR研究。 SSDNP的潜力从该技术的能力到 通过O（102-103）倍数增强自旋极化。该信号增益与O（101）倍的热极化增益相结合 从冷却到液体氮温度，O（102）从冷却到液态氦温度， 磁场为SSNMR提供多达O（105）的总信号增益，因此，实验时间减少了 直至该信号增益的平方。信号增强的这种戏剧性磁性使前所未有的SSNMR 以前对基于NMR的结构研究无法访问的样品和条件类型的研究。 在启用SSDNP的研究亮点中，有整体细胞中的膜蛋白系统的研究或研究 淀粉样纤维的第四纪结构的链间结构。我们发展的特别重点是 通过SSDNP增强的冻结蛋白质的SSDNP增强MAS NMR的聚集蛋白的瞬时结构研究 在聚集的各个阶段。 SSDNP在公认的作用中提高MAS NMR作为最终的高级 解决结构生物学工具以捕获短暂发展的结构，我们建议解决主要技术 我们创新的工具发展挑战。我们开发的核心将是一个紧凑而多功能的 带有新颖的两频泵，并发DNP和EPR以及Eldor功能的准精光桥设计 在MAS操作下。而SSDNP增强的MAS NMR是当代NMR的重点中心，因为它具有 改变生物固体的MAS NMR结构研究的潜力，只有少数替代SSDNP MAS NMR仪器 世界上存在于商业陀螺仪驱动的SSDNP MAS NMR仪器> 100 Kelvin的仪器 - 我们 DNP增强MAS NMR的仪器平台旨在提供具有更大多功能性和更大多功能性的替代解决方案 表现。