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Related Concept Videos

2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis.
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

Homonuclear correlation spectroscopy, or COSY, is a 2-dimensional NMR technique that provides information about coupled protons. Typically, the geminal and vicinal coupling are observed. For example, consider the COSY spectrum of ethyl acetate, where its 1D proton NMR spectrum is plotted along the vertical and horizontal axes with their corresponding chemical shift scale. Three spots on the diagonal corresponding to the three peaks in the 1D proton spectrum are called diagonal peaks. The COSY...
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

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.
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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 slanted or...

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Related Experiment Video

Updated: Jun 13, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

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

Published on: September 17, 2017

2H-DNP-enhanced 2H-13C solid-state NMR correlation spectroscopy.

Thorsten Maly1, Loren B Andreas, Albert A Smith

  • 1Francis Bitter Magnet Laboratory and Department of Chemistry, Cambridge, MA 02139, USA.

Physical Chemistry Chemical Physics : PCCP
|May 12, 2010
PubMed
Summary
This summary is machine-generated.

Perdeuteration of biological macromolecules combined with dynamic nuclear polarization significantly enhances magic angle spinning solid-state NMR spectra. This novel approach provides a 700-fold signal boost for (2)H-(13)C correlation spectra of proline.

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

Published on: February 12, 2019

Related Experiment Videos

Last Updated: Jun 13, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

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

Published on: September 17, 2017

Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
09:37

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

Published on: February 12, 2019

Area of Science:

  • Biophysical Chemistry
  • Structural Biology
  • Nuclear Magnetic Resonance Spectroscopy

Background:

  • Magic Angle Spinning (MAS) Solid-State Nuclear Magnetic Resonance (NMR) spectroscopy is crucial for determining the structure of biological macromolecules.
  • Perdeuteration of samples is a key technique to obtain high-resolution (2)H-(13)C correlation spectra.
  • Dynamic Nuclear Polarization (DNP) is an emerging technique for signal enhancement in NMR.

Purpose of the Study:

  • To investigate the application of (2)H-DNP for enhancing MAS solid-state NMR spectra of biological systems.
  • To evaluate the signal enhancement achieved by combining sample deuteration with DNP.
  • To obtain high-resolution (2)H-(13)C correlation spectra of a biologically relevant molecule, proline.

Main Methods:

  • Perdeuteration of U-labeled proline to incorporate deuterium and carbon-13.
  • Application of Dynamic Nuclear Polarization (DNP) with various polarizing agents.
  • Acquisition of (2)H-(13)C correlation spectra using MAS solid-state NMR with and without DNP (microwaves on/off).

Main Results:

  • Achieved a signal enhancement factor (epsilon) greater than or equal to 700 for (2)H-(13)C correlation spectra.
  • Demonstrated the first-time use of (2)H-DNP to enhance MAS-NMR spectra of a biologically relevant system.
  • Obtained resolved (2)H-(13)C correlation spectra of perdeuterated proline.

Conclusions:

  • The combination of sample deuteration and DNP is a powerful method for signal enhancement in MAS solid-state NMR.
  • This technique significantly improves spectral resolution and sensitivity for structural biology studies.
  • (2)H-DNP offers a substantial advantage for analyzing complex biological molecules like proline.