An Integrated THz System for DNP-enhanced NMR Spectroscopy

用于 DNP 增强核磁共振波谱学的集成太赫兹系统

• 批准号: 8849046
• 负责人: Thorsten Maly
• 金额: $ 51.5万
• 依托单位: BRIDGE 12 TECHNOLOGIES, INC.
• 依托单位国家: 美国
• 财政年份: 2013
• 资助国家: 美国
• 起止时间: 2013-09-05 至 2016-08-31
• 项目状态: 已结题
• 来源: https://reporter.nih.gov/project-details/8849046
• 关键词: Academia; Analytical Chemistry; Area; Cell Nucleus; Complex; Cost Savings; Crystallography; Data Quality; Development; Devices; Discipline; Drug Industry; Electrons; Foundations; Frequencies; Funding; Future; Health; Hour; Individual; Industry; Lead; Magic; Magnetism; Marketing; Measurement; Mechanics; Methods; NMR Spectroscopy; Nuclear; Optics; Output; Performance; Pharmacologic Substance; Phase; Physiologic pulse; Process; Research; Research Personnel; Research Project Grants; Resolution; Sampling; Scientist; Signal Transduction; Solutions; Source; Structure; System; Technology; Time; Tube; United States National Institutes of Health; Work; base; cold temperature; cost; design; improved; innovation; instrumentation; interest; irradiation; macromolecule; magnetic field; novel; operation; performance tests; programs; protein structure; research study; solid state nuclear magnetic resonance; structural biology; tool

DESCRIPTION (provided by applicant): The proposed research focuses on the development of a DNP-NMR system for Dynamic Nuclear Polarization (DNP) enhanced solid-state NMR spectroscopy at 400 MHz. High-resolution structures are essential to the understanding of the complex functions of bio-macromolecules and NMR spectroscopy is a major source for such information. However, the method suffers from an inherently low sensitivity and long acquisition times are required to achieve sufficient data quality. DNP, a method in which the high, thermal electron polarization is transferred to surrounding nuclei by THz irradiation of the sample, can boost the NMR sensitivity by two or three orders of magnitude. With DNP, experiments that typically require days or weeks of signal averaging can be performed in minutes or hours. It enables researchers to do experiments that are otherwise impossible to perform, such as high-precision distance measurements or recording 2D 13C-13C correlation spectra of unlabeled molecules in just hours. In this proposal we present a novel 400 MHz DNP system based on a 263 GHz gyrotron source that is integrated into the NMR magnet. Our product does not require an additional, expensive superconducting magnet. This is possible, because current (wide-bore) NMR magnets provide sufficient space right above the probe to integrate and operate the gyrotron source. This innovative gyrotron tube is specifically designed for DNP applications, provides sufficient power and has adequate frequency tuning bandwidth to eliminate the superconducting sweep coil that is necessary in other DNP systems. The presented innovations result in cost savings of >$ 0.8 million per unit and will make DNP a much more affordable method. During Phase I we will perform the mechanical and electrical design of the 263 GHz integrated THz source and select a cavity trim coil magnet assembly based on its NMR performance. During Phase II the gyrotron source will be fabricated and the complete DNP system including the low-temperature NMR probe will be integrated in the 400 MHz NMR magnet. As a result of this project, we expect a complete 400 MHz DNP system based on Bridge12's integrated gyrotron source and we expect signal enhancements of >100 in routine measurements. Although the product is initially targeted towards an academic market we expect that it will lay the foundation for a much broader acceptance of the technology in academia and industry and will bring the benefits of DNP to a much broader scientific audience.

描述（由申请人提供）：拟议的研究重点是开发 DNP-NMR 系统，用于 400 MHz 下的动态核极化 (DNP) 增强固态 NMR 光谱。高分辨率结构对于理解生物大分子的复杂功能至关重要，而核磁共振波谱是此类信息的主要来源。然而，该方法固有的灵敏度较低，并且需要较长的采集时间才能获得足够的数据质量。 DNP 是一种通过样品的太赫兹辐射将高热电子极化转移到周围原子核的方法，可以将 NMR 灵敏度提高两个或三个数量级。借助 DNP，通常需要几天或几周的信号平均的实验可以在几分钟或几小时内完成。它使研究人员能够进行原本无法进行的实验，例如高精度距离测量或在短短几小时内记录未标记分子的 2D 13C-13C 相关光谱。在本提案中，我们提出了一种新型 400 MHz DNP 系统，该系统基于集成到 NMR 磁体中的 263 GHz 回旋管源。我们的产品不需要额外的昂贵的超导磁体。这是可能的，因为当前（大口径）NMR 磁体在探头正上方提供了足够的空间来集成和操作回旋管源。这种创新的回旋管专为 DNP 应用而设计，可提供足够的功率并具有足够的频率调谐带宽，以消除其他 DNP 系统中所需的超导扫描线圈。所提出的创新可节省每单位 80 万美元以上的成本，并使 DNP 成为一种更加经济实惠的方法。在第一阶段，我们将进行 263 GHz 集成太赫兹源的机械和电气设计，并根据 NMR 性能选择腔体调整线圈磁体组件。在第二阶段，将制造回旋管源，并将包括低温 NMR 探头在内的完整 DNP 系统集成到 400 MHz NMR 磁体中。作为该项目的结果，我们期望基于 Bridge12 集成回旋管源的完整 400 MHz DNP 系统，并且我们期望在常规测量中信号增强 >100。尽管该产品最初面向学术市场，但我们预计它将为学术界和工业界更广泛地接受该技术奠定基础，并将 DNP 的优势带给更广泛的科学受众。