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相关概念视频

¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)

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When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
1.6K
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

1.4K
The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse....
1.4K
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

1.7K
A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied...
1.7K
Proton (¹H) NMR: Chemical Shift01:07

Proton (¹H) NMR: Chemical Shift

3.1K
Organic molecules primarily contain carbon and hydrogen atoms. While all the hydrogen isotopes are NMR-active, protium or hydrogen-1 is the most abundant. It has a significant energy separation between its nuclear spin states due to its large gyromagnetic ratio. As per Boltzmann's distribution, an increase in the energy separation implies a greater excess population of nuclei available for excitation, resulting in a strong NMR absorption signal.
Absorption signals of all the protium nuclei...
3.1K
¹H NMR of Labile Protons: Deuterium (²H) Substitution00:48

¹H NMR of Labile Protons: Deuterium (²H) Substitution

1.3K
This lesson illustrates the role of deuterium substitution in simplifying the NMR spectrum of compounds comprising labile protons. One method employed is the use of deuterium. Amongst the three isotopes of hydrogen, deuterium (2H) has a nucleus composed of one proton and one neutron. When the D2O solvent is added to a pure dry ethanol solution, its labile proton is substituted with deuterium.
1.3K
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.4K
Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are...
1.4K

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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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通过DNP增强的甲基固态NMR光谱探索蛋白质结构

Jiafei Mao1,2, Victoria Aladin2,3,4, Xinsheng Jin5

  • 1Institute of Biophysical Chemistry , Goethe University Frankfurt , 60438 Frankfurt am Main , Germany.

Journal of the American Chemical Society
|November 23, 2019
PubMed
概括
此摘要是机器生成的。

这项研究引入了一种新的基于甲基的工具包,用于使用动态核极化 (DNP) 增强的固态NMR (ssNMR) 进行蛋白质结构分析. 这种方法使用甲基作为传感器和"NMR火"来揭示蛋白质包装和连接位.

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Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
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科学领域:

  • 生物物理
  • 结构生物学
  • 光谱学

背景情况:

  • 动态核极化 (DNP) 显著提高了固态NMR (ssNMR) 的灵敏度,使得应用范围更广.
  • 为了在复杂的生物系统中充分利用DNP-ssNMR,进一步的方法进步至关重要.
  • 现有的ssNMR方法在探测特定分子环境和短距离结构信息方面存在局限性.

研究的目的:

  • 使用DNP-ssNMR开发一种基于甲基的新型工具包来确定蛋白质结构.
  • 用甲基作为动态传感器和"NMR火"来探测蛋白质结构和功能.
  • 扩大ssNMR研究膜蛋白等大型生物分子的能力.

主要方法:

  • 用于信号增强的DNP与异质核Overhauser效应 (hetNOE) 和碳-碳旋转扩散 (SD) 的集成.
  • 同位素标记方案的战略设计,以最大限度地利用甲基组的信息.
  • 用C-13旋转扩散来探测亚纳米距离.

主要成果:

  • 甲基组有效地探测局部分子包装,并作为"NMR火"来照亮特定区域,例如联体结合口袋.
  • C-13旋转扩散方法弥合了传统ssNMR和EPR光谱之间的分辨率差距.
  • 在大型膜蛋白绿色蛋白素 (GPR) 上证明适用性,为其光循环机制提供了洞察力.

结论:

  • 开发的基于甲基的DNP-ssNMR工具包为蛋白质结构和动态分析提供了强大的新方法.
  • 甲基是了解蛋白质结构和功能部位的多功能探针.
  • 这种方法增强了大型和复杂的生物系统的研究,包括膜蛋白.