Acquisition of 500 MHz NMR Spectrometer for High Resolution Solution Studies

采购 500 MHz NMR 波谱仪用于高分辨率溶液研究

• 批准号: 9601705
• 负责人: Peter Gettins
• 金额: $ 35万
• 依托单位: University of Illinois at Chicago
• 依托单位国家: 美国
• 项目类别: Standard Grant
• 财政年份: 1996
• 资助国家: 美国
• 起止时间: 1996-08-01 至 1998-07-31
• 项目状态: 已结题
• 来源: https://www.nsf.gov/awardsearch/showAward?AWD_ID=9601705&HistoricalAwards=false
• 关键词: Acquisition; 500; MHz; NMR; Spectrometer

Introduction For the ten research projects described here, the role of NMR spectroscopy ranges from an extremely useful complement to other spectroscopic and biochemical approaches to being the sine qua non for accomplishment of the project specific aims. In each case, however, a sophisticated, sensitive, high-field spectrometer is essential for the NMR components of the project. Such equipment is not available at the University of Illinois at Chicago (UIC) and this situation has led either to an interruption of on-going projects, to acquisition of data on a limited scale elsewhere, or to an external collaboration as a default. This is clearly unacceptable for a major Research I university such as UIC and must be urgently remedied. This proposal for a new 500MHz NMR spectrometer to be used for solution structural studies on proteins, peptides and complex natural products therefore represents part of a broader plan to address the major deficits in NMR spectroscopic facilities at UIC. The second part of the plan, to be dealt with separately, is to acquire additional NMR instrumentation equally-focussed to satisfy the needs of solids researchers. This two-pronged strategy was partly prompted by very sensible reviewers' comments on an earlier unsuccessful proposal to NSF-ARI for a 600MHz spectrometer. That single instrument proposal attempted to satisfy both solids and bio-macromolecule researchers. We think that the present bipartite, focussed-use strategy is both a more cost effective and efficient one. Proposed Instrumentation We are requesting 50% matching funds for the purchase of a narrow bore 500MHz NMR spectrometer optimized for solution structural studies on low concentrations of bio-macromolecules and complex plant-derived natural products. The spectrometer will consist of: 1. Basic two-RF channel (with lock) 500MHz spectrometer and standard bore ( 52mm) superconducting magnet with host computer and software, temperature control unit and vibration damping unit. 2. Additional two RF channels and 2H-decoupling hardware. 3. 5mm pulsed field gradient inverse triple resonance (13C and l5N) and inverse broadband (15N to 31P) probes. 5mm 19F-lH dual probe. 4. Additional temperature stabilization unit to give control of better than 0.1 C. Price quotes have been received from the two major vendors, Bruker and Varian. Although a detailed budget has been written for Bruker (p 31), the choice of instrument will be based principally on comparative performance, in addition to other considerations such as cost and future technical and equipment support. All available instruments will be evaluated. Research and Training to be Conducted The research to be conducted all relates to NMR solution structural studies on biomolecules. The studies fall into two main categories. (i) Structure elucidation of medium sized proteins, protein domains, and their complexes with DNA, with other protein domains and with peptide or polysaccharide ligands. Such studies benefit from the highestfield, most sensitive and experimentally-versatile spectrometer available. (ii) Structure elucidation of novel complex plant-derived natural products, which requires the sensitivity of a 500MHz spectrometer and the versatility of an instrument with up-to-date multi-channel pulse capabilities. Both graduate students and postdoctoral fellows will be trained in the theory and application of modern NMR spectroscopy by the core of six investigators with expertise in NMR spectroscopic methods. A joint bi-weekly NMR users research meeting is planned as a forum for dissemination of new methods and critical evaluation of acquired results. Activity resulting from funding State-of-the-art high field NMR instrumentation will have a profound and positive effect on structural research on campus. In addition to permitting the successful completion of on-going projects it will allow researchers who must now go elsewhere to carry out their studies on campus. This in turn will increase the local visibility of structurally-oriented research and help both in recruitment of structurally-oriented faculty, postdocs and students, and in fostering collaborations between faculty within the university.

对于这里描述的十个研究项目，核磁共振波谱的作用范围从对其他光谱和生化方法的极其有用的补充到实现项目特定目标的必要条件。然而，在每一种情况下，一个复杂、灵敏的高场光谱仪对于该项目的核磁共振组件都是必不可少的。伊利诺伊大学芝加哥分校(UIC)没有这种设备，这种情况要么导致正在进行的项目中断，要么导致在其他地方获得有限规模的数据，要么导致默认的外部合作。对于像UIC这样的研究型I主要大学来说，这显然是不可接受的，必须紧急补救。因此，关于将一台新的500 MHz核磁共振光谱仪用于蛋白质、多肽和复杂天然产品的溶液结构研究的建议，是解决UIC核磁共振光谱分析设施主要缺陷的更广泛计划的一部分。计划的第二部分，将单独处理，是获得额外的核磁共振仪器，同样专注于满足固体研究人员的需求。这一双管齐下的战略在一定程度上是因为非常明智的评论家对早些时候向NSF-ARI提出的600 MHz光谱仪的不成功提议发表了评论。这一单一的仪器提议试图同时满足固体和生物大分子研究人员的要求。我们认为，目前的两方集中使用战略既是一种更具成本效益的战略，也是一种更有效率的战略。建议的仪器我们正在申请50%的配套资金，用于购买一台窄口径500 MHz核磁共振光谱仪，该光谱仪针对低浓度生物大分子和复杂的植物来源天然产品的溶液结构研究进行了优化。该光谱仪由以下部分组成：1.基本双射频通道(带锁)500 MHz光谱仪和标准口径(52 Mm)超导磁体，配有上位机和软件、温度控制单元和减振单元。2.增加两个射频通道和2H去耦合硬件。3.5 mm脉冲场梯度反向三重共振(13C和15N)和反向宽带(15N到31P)探头。5 mm 19F-LH型双探头。4.已收到布鲁克和瓦里安这两家主要供应商提供的报价，可提供优于0.1摄氏度的额外温度稳定装置。虽然已经为Bruker制定了详细的预算(第31页)，但工具的选择将主要基于比较性能，以及其他考虑因素，如成本和未来的技术和设备支持。将对所有可用的工具进行评估。将要进行的研究和培训将要进行的研究都与生物分子的核磁共振溶液结构研究有关。这些研究主要分为两大类。(I)中等大小的蛋白质、蛋白质结构域及其与DNA、与其他蛋白质结构域以及与多肽或多糖配体的复合体的结构鉴定。这样的研究得益于现有的最高场强、最灵敏和实验用途最广的光谱仪。(2)新的复杂植物天然产物的结构鉴定，这需要500兆赫光谱仪的灵敏度和具有最新多通道脉冲能力的仪器的多功能性。研究生和博士后研究员都将接受现代核磁共振波谱理论和应用方面的培训，培训的核心是拥有核磁共振波谱方法专业知识的六名研究人员。计划每两周举行一次核磁共振用户联合研究会议，作为传播新方法和对已有成果进行批判性评估的论坛。资助最先进的高场核磁共振仪器所产生的活动将对校园结构研究产生深远和积极的影响。除了允许正在进行的项目的成功完成外，它还将允许现在必须到其他地方的研究人员在校园内开展他们的研究。这反过来将提高以结构为导向的研究在当地的能见度，并有助于招聘以结构为导向的教师、博士后和学生，以及促进大学内部教师之间的合作。