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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...
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...
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...
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved in...

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NMR 15N Relaxation Experiments for the Investigation of Picosecond to Nanoseconds Structural Dynamics of Proteins
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Gradient and sensitivity enhanced multiple-quantum coherence in heteronuclear multidimensional NMR experiments.

X M Kong1, K H Sze, G Zhu

  • 1Department of Biochemistry, Hong Kong University of Science and Technology, Clear Water Bay, Kowloon.

Journal of Biomolecular NMR
|November 17, 2010
PubMed
Summary
This summary is machine-generated.

Nuclear magnetic resonance (NMR) experiments utilizing multiple-quantum coherence transfer show enhanced sensitivity for studying biomolecules. This novel approach improves spectral resolution and detection limits in protein and nucleic acid analysis.

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Area of Science:

  • Biophysical Chemistry
  • Structural Biology
  • Nuclear Magnetic Resonance Spectroscopy

Background:

  • Multiple-quantum coherence (MQC) in nuclear magnetic resonance (NMR) exhibits slower relaxation rates compared to single-quantum coherence (SQC) for specific molecular sites.
  • This property has led to the development of heteronuclear NMR experiments employing MQC transfer for improved sensitivity and resolution.

Purpose of the Study:

  • To introduce and validate a novel constant-time, gradient, and sensitivity-enhanced heteronuclear multiple-bond correlation (HMQC) experiment (CT-g/s-HMQC).
  • To demonstrate the superior sensitivity of the CT-g/s-HMQC experiment compared to existing HMQC and HSQC methods.

Main Methods:

  • Development and application of a constant-time, gradient, and sensitivity-enhanced HMQC (CT-g/s-HMQC) experiment.
  • Testing the experiment on a 13C and 15N labeled calmodulin sample in D2O.
  • Extension of the MQC transfer approach to 3D NOESY-HMQC and doubly sensitivity-enhanced TOCSY-HMQC experiments.

Main Results:

  • The CT-g/s-HMQC experiment demonstrated significant sensitivity enhancement over standard constant-time HMQC.
  • The CT-g/s-HMQC also showed greater sensitivity compared to constant-time gradient and sensitivity-enhanced HSQC (CT-g/s-HSQC) experiments.
  • The adapted 3D NOESY-HMQC and doubly sensitivity-enhanced TOCSY-HMQC experiments were found to be more sensitive than their HSQC counterparts.

Conclusions:

  • The developed CT-g/s-HMQC experiment offers a substantial increase in sensitivity for NMR studies of biomolecules.
  • Utilizing multiple-quantum coherence transfer in heteronuclear NMR experiments provides a viable strategy for enhancing spectral quality and detection limits.