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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

基本信息

批准号：
8921222
负责人：
Thorsten Maly
金额：
$ 45.12万
依托单位：
BRIDGE 12 TECHNOLOGIES, INC.
依托单位国家：
美国
项目类别：
财政年份：
2013
资助国家：
美国
起止时间：
2013-09-05 至 2017-08-31
项目状态：
已结题

来源：
https://reporter.nih.gov/project-details/8921222
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

项目摘要

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）：拟议的研究重点是在400 MHz下开发用于动态核极化（DNP）增强固态NMR光谱的DNP-NMR系统。高分辨率结构对于理解生物大分子的复杂功能是必不可少的，并且NMR光谱是这些信息的主要来源。然而，该方法具有固有的低灵敏度，并且需要长的采集时间来实现足够的数据质量。DNP是一种通过太赫兹辐射样品将高热电子极化转移到周围原子核的方法，可以将NMR灵敏度提高两到三个数量级。使用DNP，通常需要数天或数周信号平均的实验可以在几分钟或几小时内完成。它使研究人员能够在短短几个小时内完成其他方法无法完成的实验，例如高精度距离测量或记录未标记分子的2D 13 C-13 C相关光谱。在这个建议中，我们提出了一种新的400 MHz的DNP系统的基础上，263 GHz的回旋管源，集成到NMR磁体。我们的产品不需要额外的、昂贵的超导磁体。这是可能的，因为当前的（宽孔）NMR磁体在探针上方提供了足够的空间来集成和操作回旋管源。这种创新的回旋管是专门为DNP应用而设计的，提供足够的功率，并具有足够的频率调谐带宽，以消除超导扫描线圈，这是必要的其他DNP系统。所提出的创新导致每单位成本节省> 80万美元，并将使DNP成为一种更实惠的方法。在第一阶段，我们将进行机械和电气设计的263 GHz的集成太赫兹源，并选择一个腔修剪线圈磁铁组件的基础上，其NMR性能。在第二阶段，回旋管源将被制造和完整的DNP系统，包括低温核磁共振探针将被集成在400兆赫核磁共振磁铁。作为这个项目的结果，我们期望一个完整的400 MHz DNP系统的基础上桥12的集成回旋管源，我们希望在常规测量信号增强>100。虽然该产品最初针对的是学术市场，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的好处带给更广泛的科学受众。