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）：拟议的研究重点是开发DNP-NMR动态核极化系统（DNP）在400 MHz时增强了固态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NMR光谱是此类信息的主要来源。但是，该方法具有固有的低灵敏度，需要长时间的获取时间才能达到足够的数据质量。 DNP是一种通过样品的THZ照射将高热电子极化转移到周围核的方法，可以将NMR灵敏度提高两个或三个数量级。对于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个小时内进行。它使研究人员能够进行原本无法执行的实验，例如高精度距离测量或记录2d 13c-13c相关光谱，即仅在短短几个小时内。在此提案中，我们提出了一个新型的400 MHz DNP系统，该系统基于集成到NMR磁铁中的263 GHz旋转源。我们的产品不需要额外的，昂贵的超导磁铁。这是可能的，因为电流（宽孔）NMR磁体在探针上方提供足够的空间以整合和操作陀螺仪源。这种创新的旋转管专为DNP应用而设计，提供足够的功率并具有足够的频率调整带宽，以消除其他DNP系统中必需的超导扫描线圈。提出的创新导致每单位的成本节省> 80万美元，并且将使DNP成为更实惠的方法。在第一阶段，我们将执行263 GHz集成THZ源的机械和电气设计，并根据其NMR性能选择一个空腔装饰线圈组件。在II期期间，将制造循环源，并将包括低温NMR探针（包括低温NMR探针）集成在400 MHz NMR磁铁中。该项目的结果是，我们希望基于Bridge12的集成循环源建立完整的400 MHz DNP系统，并希望在常规测量中提高> 100的信号增强。尽管该产品最初是针对学术市场的，但我们希望它将为在学术界和行业中更广泛接受该技术的基础奠定基础，并将DNP的好处带给更广泛的科学受众。