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Related Concept Videos

Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by...
274
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.1K
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...
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Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

820
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....
820
NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences01:17

NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences

893
A pulse is a short burst of radio waves distributed over a range of frequencies that simultaneously excites all the nuclei in the sample. Upon passing a radio frequency pulse along the x-axis, the nuclei absorb energy corresponding to their Larmor frequencies and achieve resonance. This shifts the net magnetization vector from the z-axis toward the transverse plane. This angle of rotation of the magnetization vector, or the flip angle, is proportional to the duration and intensity of the pulse.
893
Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)01:15

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)

469
Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) is an advanced Nuclear Magnetic Resonance (NMR) technique specifically designed to detect and enhance the signals of low-abundance nuclei, such as carbon-13 and nitrogen-15, in small molecules. The fundamental principle behind INEPT is the transfer of polarization from a more abundant and highly polarizable nucleus, typically hydrogen-1, to the low-abundance nucleus of interest. This process effectively boosts the NMR signal of the...
469
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

765
When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...
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Quantifying Mixing using Magnetic Resonance Imaging
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Sensitivity-Enhanced Multidimensional Solid-State NMR Spectroscopy by Optimal-Control-Based Transverse Mixing

Jan Blahut1,2, Matthias J Brandl3, Tejaswini Pradhan3

  • 1Department of Chemistry, Faculty of Science, Charles University, Albertov 6, 12842 Prague, Czech Republic.

Journal of the American Chemical Society
|September 8, 2022
PubMed
Summary
This summary is machine-generated.

Proton-detected solid-state NMR experiments were enhanced using novel transverse mixing sequences. This improved signal-to-noise ratio, enabling the characterization of previously undetectable protein structures.

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Area of Science:

  • Biophysical Chemistry
  • Structural Biology
  • Spectroscopy

Background:

  • Proton-detected magic-angle spinning (MAS) solid-state NMR spectroscopy is crucial for studying insoluble protein structure and dynamics.
  • Existing multidimensional NMR experiments can be improved by simultaneously transferring transversal magnetization components.
  • Preservation of equivalent pathways (PEP) in solution NMR faces limitations due to relaxation in larger molecules.

Purpose of the Study:

  • To develop and implement novel heteronuclear transverse mixing sequences for correlation experiments in solid-state NMR.
  • To enhance the signal-to-noise ratio (SNR) in proton-detected multidimensional NMR experiments.
  • To enable the atomic-resolution characterization of challenging protein samples, such as minor fibril polymorphs.

Main Methods:

  • Development of heteronuclear transverse mixing sequences optimized using optimal control theory for moderate and fast MAS frequencies.
  • Implementation of a carbon-detected, sensitivity-enhanced 2D NCA experiment.
  • Design and application of a novel proton-detected, doubly sensitivity-enhanced 3D hCANH pulse sequence.

Main Results:

  • Optimal control significantly boosted the signal-to-noise ratio (SNR) beyond theoretical expectations.
  • A 3-fold SNR improvement was observed for the novel 3D hCANH pulse sequence compared to conventional methods.
  • The enhanced sensitivity allowed for the unambiguous characterization of a minor fibril polymorph of human lambda-III immunoglobulin light chain protein.

Conclusions:

  • The developed transverse mixing sequences provide a substantial sensitivity gain for proton-detected solid-state NMR.
  • These advanced NMR techniques are essential for overcoming sensitivity limitations in studying complex biological systems.
  • The study successfully characterized a previously undetected protein fibril polymorph, highlighting the power of enhanced solid-state NMR.