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Related Concept Videos

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

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

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

Two-Dimensional (2D) NMR: Overview

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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....
1.3K
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

553
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...
553
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

668
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...
668
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

1.8K
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...
1.8K
NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences01:17

NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences

1.6K
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.
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Single-throughput Complementary High-resolution Analytical Techniques for Characterizing Complex Natural Organic Matter Mixtures
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Fast quantitative 2D NMR for metabolomics and lipidomics: A tutorial.

Estelle Martineau1,2, Jean-Nicolas Dumez1, Patrick Giraudeau1,3

  • 1CEISAM, CNRS UMR 6230, Université de Nantes, Nantes, France.

Magnetic Resonance in Chemistry : MRC
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Summary

Nuclear magnetic resonance (NMR) provides quantitative analysis for metabolomics and lipidomics. Fast 2D NMR methods improve spectral resolution and reduce experiment time for complex biological samples.

Keywords:
2D NMR spectroscopyfast methodslipidomicsmetabolomicsquantitative analysistargeteduntargeted

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Area of Science:

  • Analytical Chemistry
  • Biochemistry
  • Spectroscopy

Background:

  • Nuclear magnetic resonance (NMR) is a powerful analytical technique for complex mixture analysis.
  • Its quantitative capabilities are valuable for metabolomics and lipidomics studies.
  • Spectral overcrowding in 1D NMR spectra is a significant limitation for complex biological samples.

Purpose of the Study:

  • To describe a general workflow for acquiring fast quantitative 2D NMR spectra in omics studies.
  • To demonstrate the application of fast acquisition methods to overcome spectral overcrowding.
  • To provide recommendations for implementing these protocols in metabolomics and lipidomics.

Main Methods:

  • Utilized 2D NMR spectroscopy for enhanced spectral separation and quantitative accuracy.
  • Employed fast acquisition methods to reduce experiment duration.
  • Illustrated the workflow using Uniform Sampling COrrelated SpectroscopY (UF COSY), Zero-Filling Total Correlation SpectroscopY (ZF-TOCSY) with nonuniform sampling, and Heteronuclear Single Quantum Coherence (HSQC) with nonuniform sampling.

Main Results:

  • Demonstrated that 2D NMR spectra provide better separation of overlapped resonances compared to 1D NMR.
  • Showcased the ability to obtain accurate quantitative data with appropriate analytical protocols.
  • Successfully reduced experiment duration through fast acquisition techniques.

Conclusions:

  • Fast quantitative 2D NMR is a viable approach for omics studies.
  • The described workflow facilitates efficient analysis of complex biological samples.
  • This methodology supports both targeted and untargeted metabolomics and lipidomics investigations.