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Related Concept Videos

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

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

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...
Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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...

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Real-Time Metabolic Detection in Living Cells Using Hyperpolarized 13C NMR
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Hyperpolarized Hadamard spectroscopy using flow NMR.

Hsueh-Ying Chen1, Christian Hilty

  • 1Department of Chemistry, Texas A&M University, 3255 TAMU, College Station, TX 77843-3255, USA.

Analytical Chemistry
|July 10, 2013
PubMed
Summary
This summary is machine-generated.

This study introduces multiscan spectroscopy for dissolution dynamic nuclear polarization (D-DNP) NMR, enabling powerful correlation experiments. This breakthrough enhances D-DNP

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Area of Science:

  • Nuclear Magnetic Resonance Spectroscopy
  • Hyperpolarization Techniques

Background:

  • Dissolution dynamic nuclear polarization (D-DNP) significantly enhances NMR signal sensitivity.
  • The single-scan nature of D-DNP limits its application in complex correlation spectroscopy.
  • Correlation NMR experiments are crucial for detailed molecular structure elucidation.

Purpose of the Study:

  • To develop a multiscan spectroscopy method for D-DNP samples.
  • To enable chemical shift correlation experiments using D-DNP.
  • To increase the versatility of D-DNP for small-molecule characterization.

Main Methods:

  • Utilizing a flow NMR probe for sequential injection of hyperpolarized sample segments.
  • Applying Hadamard spectroscopy for data acquisition from multiple scans.
  • Developing an entropy-based maximization procedure for Hadamard reconstruction, accounting for relaxation and concentration gradients.

Main Results:

  • Demonstrated [(13)C,(1)H] correlation spectroscopy on 1-butanol using a four-scan dataset.
  • Successfully obtained chemical shift correlation information from a limited number of scans.
  • Developed a robust reconstruction method for multiscan D-DNP data.

Conclusions:

  • Multiscan NMR spectroscopy is a viable approach for D-DNP samples.
  • This method expands the applicability of D-DNP to correlation NMR experiments.
  • The technique enhances the utility of D-DNP in characterizing small molecules.