Name: high-sensitivity nuclear magnetic resonance at giga-pascal pressures: a new tool for probing electronic and chemical properties of condensed matter under extreme conditions
Uploaded: 2014-10-10T15:00:00.000+00:00
Duration: 8 min 42 s
Description: Watch this Scientific Journal Video about High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extr

This research was funded by the International Research Training Group (IRTG) &#8220;Diffusion in porous Materials&#8221;. We acknowledge the technical support from Gert Klotzsche and stimulating discussions with Steven Reichhardt, Thomas Meissner, Damian Rybicki, Tobias Herzig, Natalya Georgieva, Jonas Kohlrautz, and Michael Jurkutat.

1，安装和6H-SiC的大锥伯勒尔型砧的对齐<ol><li>修正了在安装工具活塞和XY板插入伯勒尔型砧的休息区。 </li><li>确保每个砧坐在稳稳的背板。 </li><li>采用环氧树脂，（ 例如 ，STYCAST 1266），胶砧均向自己的座位上。固化在室温下12小时，或65ºC在炉中2小时。 </li><li>为了有足够的铁砧对齐，用货币供应量M1止动螺钉对齐背板和监控两个砧的并行性。如果被发现的砧块是不平行的，除去环氧树脂和重新启动点1.2处。 </li></ol> 2垫片准备<ol><li>钻头1毫米的孔进入退火铜成为一个芯片（铜98瓦特％，为2％（重量），厚度为0.5mm）的黄铜导销。 </li><li>插入三个长5mm条直径为1毫米的非绝缘铜线插入孔中，这是沿着砧分布，以作为GUIDË引脚的铜要垫片。 </li><li>检查之间的导销和胞体正确接地。通常情况下，约0.1Ω的直流电阻是理想的。改善与少量的导电银的应用。 </li><li>广场上的莫桑石砧顶部的铜成为芯片和关闭的单元格。 </li><li>使用油压机，加压垫片约1/8底尖直径为最大化的工作稳定性。监控用千分尺卡尺压痕的实际厚度。 </li><li>钻适当的直径（底尖直径为½）在压痕中心的孔。 </li><li>中分两个通道进入预凹垫圈。信道应足够深以容纳微线圈的18微米的铜导线。 </li><li>硬化的炉中所制备的衬垫在617 K表示2至3小时。 </li></ol> 3，准备和微线圈的加载<ol><li>采用了一块1毫米铜线的d至馈通在活塞的螺纹它。固定铜线用环氧树脂和根据步骤1.3治愈它。 </li><li>选择锥子（见材料清单），其具有用于将微线圈的所需直径和固定它的一对可旋转的卡盘夹爪之间。 </li><li>胶（ 如与清漆从SCB，见材料清单）的18微米的铜导线的一端上的卡盘爪，同时保持，另一端与旋转的卡盘爪，使得导线被卷绕到锥子。 </li><li>当微线圈是所期望的几何形状，固定金属丝的另一端部上的胶为好。 </li><li>使用稀释的清漆通过在绕组的顶部施加少量固定线圈。 </li><li>使用铁氟龙胶带锥子小心地取出线圈。 </li><li>放置一些环氧树脂（见点1.3），无任何添加剂，在密封垫的频道。 </li><li>将微线圈的样品室内部并固定在引线进入通道。 </li><li>治愈的磐英根据Ÿ树脂步骤1.3。 </li><li>焊料的微线圈的热丝，另一个导销的一个引线。 </li><li>添加一些银导电浆料每个结顶。固化过程通常需要几分钟。 </li><li>用少量环氧树脂密封两个结。 </li><li>治疗根据步骤1.3环氧树脂。 </li><li>现在，检查该线圈的直流电阻的每一步之后。 </li><li>放置在微线圈的样品。要知道，任何不必要的身体接触可能会破坏线圈。 </li><li>加入精细研磨的红宝石粉末样品的压力校准。 </li><li>最后，水灾与适当的压力介质的样品室中。用石蜡油，以确保近静水条件下可达9 GPA。 </li><li>小心合上电池。 </li></ol> 4，应用和监控压力<ol><li>起初，稍微收紧货币供应M3六角沉头螺钉。 </li><li>对于加压固定在台钳细胞。现在，拧紧两个对立的螺丝配对。 </li><li>将加压的细胞在适当的细胞支架。 </li><li>调整单元的位置，以使激光束到达样品室。 </li><li>使用精细调节表聚焦红宝石粉末在激光束。 </li><li>显示器采用相应的光谱仪软件红宝石光致发光光谱。 </li><li>提取在从红宝石R1和R2线所观察到的光谱位移的样品腔的实际压力。 </li><li>平衡加压的细胞至少12小时NMR测量前。 </li></ol> 5，执行NMR实验<ol><li>安装压力盒上典型的核磁共振探头。制造一个机械车间相应的单元格持有人。 </li><li>焊接热丝到探针。检查细胞和探针之间的适当的电接触。 </li><li>现在，执行标准NMR实验。提请注意的事实是，微线圈是版y以所施加的射频功率敏感。 </li></ol>

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The authors have nothing to disclose.

一个新的，有前途的方法，以千兆帕斯卡的压力进行核磁共振被描述。这种方法开启了大门，各种各样的NMR实验，由于其出色的灵敏度和分辨率。然而，在该协议部分中所述的几个步骤是至关重​​要的实验的结果。特别是，在制备微线圈和其在所述Cu-成为垫圈固定是非常困难的，并且需要一定的经验。在下文中，一些重要的提示被给出，这将有助于该技术的第一次成功应用。 <p class="jove_conte...

由于在上个世纪初高静水压力凝聚态珀西·布里奇曼的标志性实验，高压物理学领域已经发展迅速1。大量的有趣的现象是已知的下几个GPA 2的压力下发生。此外，凝聚态系统的高压反应已经告诉我们很多关于他们的电子基态和激发态3,4。 不幸的是，技术的凝聚态的千兆帕斯卡压力的电子性质的研究并不多见，与X射线或直流电阻测量一路领先5。特别地，电子或核磁矩与电子自旋（ESR）或核磁共振（NMR）实验中，检测被绑定到几乎不可能在一个典型的高压砧座单元，其中一个需要从检索的信号来实现一个小v通过砧座和密封垫圈olume供奉。 几个小组已尝试通过使用复杂的安排，要解决这个问题，例如，两个分割线对射频（RF）线圈沿砧块6的侧面缠绕;单或双环流发针谐振器7,8; 。甚至分裂铼垫圈作为RF拾取线圈9， 见图1不幸的是，这些方法仍然从低信号对噪声比（SNR）遭遇，限制了实验应用到大- γ核如1 H 10。有兴趣的读者可以称作其它高压谐振电路实验11 - 15。 Pravica和Silvera 16报告后的核磁共振砧细胞与12.8 GPA，谁研究了邻对位氢转换的最高压力。 随着应用核磁共振极大的兴趣研究量子固体的性质，我们集团很感兴趣，有核磁共振可在高压下，也是如此。最后，在2009年它可以证实高灵敏度砧细胞NMR的确是可能的，如果谐振无线电频率（RF）微线圈是在高压腔包围的样品17直接放置。在这样的方法中，NMR灵敏度是由几个数量级的（主要是由于急剧增加填充的RF线圈的因子），其变得更加具有挑战性NMR实验可能的， 例如在粉末样品的提高，17 O NMR高温超导体在长达7 GPA 18。超导这些材料可以通过施加压力大大放大了，现在就可以按照这个过程与当地的电子探头，承诺根本的洞察管理流程。另一实例为核磁共振高压下的功率从出现什么是believ编为常规参考实验:为了测试引入新砧细胞核磁共振，最著名的材料中的一种测定 - 简单的铝金属。随着压力的增加，从人们所期望的自由电子系统的NMR位移的一个意想不到的偏差被发现。增加下压力的反复实验，也表明新的结果确实是可靠的。最后，与带结构的计算然后将其发现的结果是，铝的费米表面，而无法通过计算年前被检测到的拓扑过渡的表现形式，在计算能力低。的调查结果的环境条件推断表明，这种金属的使用几乎无处不在的特性是由这个特殊的电子状态的影响。 为了追求许多不同的应用的特殊设计的砧座单元（前细胞已经从Cavend进口ISH实验室改造核磁共振）已经制定出来。目前，所使用自制的底盘是能够使用对800微米的底尖刻6H-SiC的砧块到达压力高至25京帕。核磁共振实验，成功地进行了高达10.1 GPa时为止。这种新的细胞的NMR性能被证明是优良19。其主要成分是钛铝（6）-Vanadium（4）与超低间隙水平（等级23），提供约800屈服强度MPa 20。由于它的非磁特性（磁化率χ是约5ppm）它是用于在砧座单元机架的适当材料。引入细胞（ 见图2中的所有自制的压腔设计概述）的整体尺寸小到足以放入普通标准孔核磁共振磁体。最小的设计中，LAC-TM1，这是只有20毫米高和1​​7毫米的直径，也符合典型的小，冷孔磁铁（30毫米孔直径）。第lAC-TM2，这是最新的底盘作者设计，使用四个M4内六角沉头螺栓（做出来的相同的合金作为电池机箱）作为压力驱动机构，允许在内部压力的平稳控制（安装在蓝图补充部分）。 通常情况下，金刚石砧使用，以便产生上述为100GPa最高压力。许茂和21 - 23已经证明，莫桑石砧提供高压的研究具有成本效益的替代方案，高达约60 GPA的压力。因此，碳硅石砧块被用于引入GPA NMR方法。最好的结果是用自Charles＆科尔瓦德的砧座部定制大锥6H-SiC的砧块。与这些细胞中，压力达10.1 GPa时使用800微米的底尖刻砧被发现导致非常好的NMR灵敏度。为了进行比较，李等人报道的1 SNR核为1 H NM自来水中的R，而引入微线圈的方法的SNR显示出25的值对于其体积的七分之一，即使在稍微较低的磁场。 有了这项新措施，以高灵敏度压腔核磁共振可以追求的承诺令人兴奋的新洞察现代材料的物理和化学多种应用。然而，一如既往的灵敏度和分辨率最终限制NMR的应用，特别是，如果一个人的爱好有高得多的压力需要小型的底尖大小。然后，人们不仅以优化电池设计具有更小的RF线圈，而且还考虑增加核极化方法。

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high-sensitivity nuclear magnetic resonance at giga-pascal pressures: a new tool for probing electronic and chemical properties of condensed matter under extreme conditions

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their electronic properties. The application of high pressure enables one to synthesize new materials, but the response of known materials to high pressure is a very useful tool for studying their electronic structure and developing theories. For example, high-pressure synthesis might be at the origin of life; and understanding the behavior of small molecules under extreme pressure will tell us more about fundamental processes in our universe. It is no wonder that there has always been great interest in having NMR available at high pressures. Unfortunately, the desired pressures are often well into the Giga-Pascal (GPa) range and require special anvil cell devices where only very small, secluded volumes are available. This has restricted the use of NMR almost entirely in the past, and only recently, a new approach to high-sensitivity GPa NMR, which has a resonating micro-coil inside the sample chamber, was put forward. This approach enables us to achieve high sensitivity with experiments that bring the power of NMR to Giga-Pascal pressure condensed matter research. First applications, the detection of a topological electronic transition in ordinary aluminum metal and the closing of the pseudo-gap in high-temperature superconductivity, show the power of such an approach. Meanwhile, the range of achievable pressures was increased tremendously with a new generation of anvil cells (up to 10.1 GPa), that fit standard-bore NMR magnets. This approach might become a new, important tool for the investigation of many condensed matter systems, in chemistry, geochemistry, and in physics, since we can now watch structural changes with the eyes of a very versatile probe.

图3示出了如何在完全组装压力盒，布线和安装到一个典型的NMR探针样子。在下文中，几个实验进行审查，应使读者能够收集有关的优点和引入的技术的范围广泛的概述。 <img alt="图1" src="/files/ftp_upload/52243/52243fig1highres.jpg" /> 图1:不同的方法适用于高压核磁共振:（一）拆分对线圈围绕砧侧面，以及从Bertani 等铼垫...

Watch this Scientific Journal Video about High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extr

High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

高灵敏度核磁共振的千兆帕斯卡压力:一种新的工具，用于极端条件下探测电子和化工凝聚态的性质

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their ...

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Principles of Nuclear Magnetic Resonance

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11.5K 次观看.  University of Leipzig. Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

视频: High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

在极端的压力和温度的合成和Microdiffraction

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

科研

工程学

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Supramolecular protein assemblies play fundamental roles in biological processes ranging from host-pathogen interaction, viral infection to the propagation of neurodegenerative disorders. Such assemblies consist in multiple protein subunits organized in a non-covalent way to form large macromolecular objects that can execute a variety of cellular functions or cause detrimental consequences. Atomic insights into the assembly mechanisms and the functioning of those macromolecular assemblies remain often scarce since their inherent insolubility and non-crystallinity often drastically reduces the quality of the data obtained from most techniques used in structural biology, such as X-ray crystallography and solution Nuclear Magnetic Resonance (NMR). We here present magic-angle spinning solid-state NMR spectroscopy (SSNMR) as a powerful method to investigate structures of macromolecular assemblies at atomic resolution. SSNMR can reveal atomic details on the assembled complex without size and solubility limitations. The protocol presented here describes the essential steps from the production of 13C/15N isotope-labeled macromolecular protein assemblies to the acquisition of standard SSNMR spectra and their analysis and interpretation. As an example, we show the pipeline of a SSNMR structural analysis of a filamentous protein assembly.

Structures of supramolecular protein assemblies at atomic resolution are of high relevance because of their crucial roles in a variety of biological phenomena. Herein, we present a protocol to perform high-resolution structural studies on insoluble and non-crystalline macromolecular protein assemblies by magic-angle spinning solid-state nuclear magnetic resonance spectroscopy (MAS SSNMR).

固体核磁共振波谱法研究高分子组件的原子尺度结构

Supramolecular protein assemblies play fundamental roles in biological processes ranging from host-pathogen interaction, viral infection to the ...

生物化学

Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR

The main limitation of NMR-based investigations is low sensitivity. This prompts for long acquisition times, thus preventing real-time NMR measurements of metabolic transformations. Hyperpolarization via dissolution DNP circumvents part of the sensitivity issues thanks to the large out-of-equilibrium nuclear magnetization stemming from the electron-to-nucleus spin polarization transfer. The high NMR signal obtained can be used to monitor chemical reactions in real time. The downside of hyperpolarized NMR resides in the limited time window available for signal acquisition, which is usually on the order of the nuclear spin longitudinal relaxation time constant, T1, or, in favorable cases, on the order of the relaxation time constant associated with the singlet-state of coupled nuclei, TLLS. Cellular uptake of endogenous molecules and metabolic rates can provide essential information on tumor development and drug response. Numerous previous hyperpolarized NMR studies have demonstrated the relevancy of pyruvate as a metabolic substrate for monitoring enzymatic activity in vivo. This work provides a detailed description of the experimental setup and methods required for the study of enzymatic reactions, in particular the pyruvate-to-lactate conversion rate in presence of lactate dehydrogenase (LDH), by hyperpolarized NMR.

The sensitivity enhancement provided by dissolution dynamic nuclear polarization (DNP) enables following metabolic processes in real time by NMR and MRI. The characteristics and performances of a dedicated dissolution DNP setup designed for study enzymatic reactions are discussed.

溶出动态核极化仪器用NMR实时酶反应速率测量

The main limitation of NMR-based investigations is low sensitivity. This prompts for long acquisition times, thus preventing real-time NMR measurements of ...

化学

High-Pressure NMR Experiments for Detecting Protein Low-Lying Conformational States

High-pressure is a well-known perturbation method that can be used to destabilize globular proteins and dissociate protein complexes in a reversible manner. Hydrostatic pressure drives thermodynamical equilibria toward the state(s) with the lower molar volume. Increasing pressure offers, therefore, the opportunities to finely tune the stability of globular proteins and the oligomerization equilibria of protein complexes. High-pressure NMR experiments allow a detailed characterization of the factors governing the stability of globular proteins, their folding mechanisms, and oligomerization mechanisms by combining the fine stability tuning ability of pressure perturbation and the site resolution offered by solution NMR spectroscopy. Here we present a protocol to probe the local folding stability of a protein via a set of 2D 1H-15N experiments recorded from 1 bar to 2.5 kbar. The steps required for the acquisition and analysis of such experiments are illustrated with data acquired on the RRM2 domain of hnRNPA1.

We provide a detailed description of the steps required to assemble a high-pressure cell, set up and record high-pressure NMR experiments, and finally analyze both peak intensity and chemical shift changes under pressure. These experiments can provide valuable insights into the folding pathways and structural stability of proteins.

检测蛋白质低洼构象状态的高压NMR实验

High-pressure is a well-known perturbation method that can be used to destabilize globular proteins and dissociate protein complexes in a reversible ...

High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

Nuclear magnetic resonance (NMR) spectroscopy represents an important technique to understand the structure and bonding environments of molecules. There exists a drive to characterize materials under conditions relevant to the chemical process of interest. To address this, in situ high-temperature, high-pressure MAS NMR methods have been developed to enable the observation of chemical interactions over a range of pressures (vacuum to several hundred bar) and temperatures (well below 0 &#176;C to 250 &#176;C). Further, the chemical identity of the samples can be comprised of solids, liquids, and gases or mixtures of the three. The method incorporates all-zirconia NMR rotors (sample holder for MAS NMR) which can be sealed using a threaded cap to compress an O-ring. This rotor exhibits great chemical resistance, temperature compatibility, low NMR background, and can withstand high pressures. These combined factors enable it to be utilized in a wide range of system combinations, which in turn permit its use in diverse fields as carbon sequestration, catalysis, material science, geochemistry, and biology. The flexibility of this technique makes it an attractive option for scientists from numerous disciplines.

The molecular structures and dynamics of solids, liquids, gases, and mixtures are of critical interest to diverse scientific fields. High-temperature, high-pressure in situ MAS NMR enables detection of the chemical environment of constituents in mixed phase systems under tightly controlled chemical environments.

高温高压原位魔角旋转核磁共振光谱

Nuclear magnetic resonance (NMR) spectroscopy represents an important technique to understand the structure and bonding environments of molecules. There ...

Paramagnetic Relaxation Enhancement for Detecting and Characterizing Self-Associations of Intrinsically Disordered Proteins

Intrinsically disordered proteins and intrinsically disordered regions within proteins make up a large and functionally significant part of the human proteome. The highly flexible nature of these sequences allows them to form weak, long-range, and transient interactions with diverse biomolecular partners. Specific yet low-affinity interactions promote promiscuous binding and enable a single intrinsically disordered segment to interact with a multitude of target sites. Because of the transient nature of these interactions, they can be difficult to characterize by structural biology methods that rely on proteins to form a single, predominant conformation. Paramagnetic relaxation enhancement NMR is a useful tool for identifying and defining the structural underpinning of weak and transient interactions. A detailed protocol for using paramagnetic relaxation enhancement to characterize the lowly-populated encounter complexes that form between intrinsically disordered proteins and their protein, nucleic acid, or other biomolecular partners is described.

A protocol for the application of paramagnetic relaxation enhancement NMR spectroscopy to detect weak and transient inter- and intra-molecular interactions in intrinsically disordered proteins is presented.

顺磁弛豫增强，用于检测和表征固有无序蛋白质的自缔合

Intrinsically disordered proteins and intrinsically disordered regions within proteins make up a large and functionally significant part of the human ...

High-Resolution Studies of Proteins in Natural Membranes by Solid-State NMR

Membrane proteins are vital for cell function and thus represent important drug targets. Solid-state Nuclear Magnetic Resonance (ssNMR) spectroscopy offers a unique access to probe the structure and dynamics of such proteins in biological membranes of increasing complexity. Here, we present modern solid-state NMR spectroscopy as a tool to study structure and dynamics of proteins in natural lipid membranes and at atomic scale. Such spectroscopic studies profit from the use of high-sensitivity ssNMR methods, i.e., proton-(1H)-detected ssNMR and DNP (Dynamic Nuclear Polarization) supported ssNMR. Using bacterial outer membrane beta-barrel protein BamA and the ion channel KcsA, we present methods to prepare isotope-labeled membrane proteins and to derive structural and motional information by ssNMR.

<meta charset="utf8"></head><body>通过固体 NMR 对天然膜中的蛋白质进行高分辨率研究

This work details robust basic routines on how to prepare isotope-labeled membrane protein samples and analyze them at high-resolution with modern solid-state NMR spectroscopy methods.

通过固体 NMR 对天然膜中的蛋白质进行高分辨率研究

Membrane proteins are vital for cell function and thus represent important drug targets. Solid-state Nuclear Magnetic Resonance (ssNMR) spectroscopy ...

<meta charset="utf8"></head><body>蛋白质动力学研究中 NMR 15N 弛豫和 hetNOE 实验的方案

NMR 15N Relaxation Experiments for the Investigation of Picosecond to Nanoseconds Structural Dynamics of Proteins

Nuclear magnetic resonance (NMR) spectroscopy allows studying proteins in solution and under physiological temperatures. Frequently, either the amide groups of the protein backbone or the methyl groups in side chains are used as reporters of structural dynamics in proteins. A structural dynamics study of the protein backbone of globular proteins on 15N labeled and fully protonated samples usually works well for proteins with a molecular weight of up to 50 kDa. When side chain deuteration in combination with transverse relaxation optimized spectroscopy (TROSY) is applied, this limit can be extended up to 200 kDa for globular proteins and up to 1 MDa when the focus is on the side chains. When intrinsically disordered proteins (IDPs) or proteins with intrinsically disordered regions (IDRs) are investigated, these weight limitations do not apply but can go well beyond. The reason is that IDPs or IDRs, characterized by high internal flexibility, are frequently dynamically decoupled. Various NMR methods offer atomic-resolution insights into structural protein dynamics across a wide range of time scales, from picoseconds up to hours. Standard 15N relaxation measurements overview a protein&#39;s internal flexibility and characterize the protein backbone dynamics experienced on the fast pico- to nanosecond timescale. This article presents a hands-on protocol for setting up and recording NMR 15N R1, R2, and heteronuclear Overhauser effect (hetNOE) experiments. We show exemplary data and explain how to interpret them simply qualitatively before any more sophisticated analysis.

<meta charset="utf8"></head><body>作者聚焦：通过 NMR 弛豫实验探索内在无序的蛋白质动力学

Nuclear magnetic resonance (NMR) spectroscopy can characterize structural protein dynamics in a residue-specific manner. We provide a hands-on protocol for recording NMR 15N R1 and R2 relaxation and {1H}-15N heteronuclear Overhauser effect (hetNOE) experiments, sensitive to the picoseconds to nanoseconds timescale.

NMR 15N 弛豫实验，用于研究蛋白质皮秒至纳秒的结构动力学

Nuclear magnetic resonance (NMR) spectroscopy allows studying proteins in solution and under physiological temperatures. Frequently, either the amide ...

高灵敏度核磁共振的千兆帕斯卡压力:一种新的工具，用于极端条件下探测电子和化工凝聚态的性质

摘要

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此视频中的章节

在极端的压力和温度的合成和Microdiffraction

固体核磁共振波谱法研究高分子组件的原子尺度结构

溶出动态核极化仪器用NMR实时酶反应速率测量

检测蛋白质低洼构象状态的高压NMR实验

高温高压原位魔角旋转核磁共振光谱

顺磁弛豫增强，用于检测和表征固有无序蛋白质的自缔合

通过固体 NMR 对天然膜中的蛋白质进行高分辨率研究

通过固体 NMR 对天然膜中的蛋白质进行高分辨率研究

NMR ¹⁵N 弛豫实验，用于研究蛋白质皮秒至纳秒的结构动力学

NMR ¹⁵N 弛豫实验，用于研究蛋白质皮秒至纳秒的结构动力学