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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...
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...
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...
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied first.

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Updated: May 24, 2026

The Identification of Sea Lamprey Pheromones Using Bioassay-Guided Fractionation
09:35

The Identification of Sea Lamprey Pheromones Using Bioassay-Guided Fractionation

Published on: July 17, 2018

Comprehensive multiphase NMR spectroscopy: basic experimental approaches to differentiate phases in heterogeneous

Denis Courtier-Murias1, Hashim Farooq, Hussain Masoom

  • 1Department of Chemistry, University of Toronto, 1265 Military Trail, Toronto, ON, Canada M1C 1A4.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|March 20, 2012
PubMed
Summary

A new Comprehensive Multiphase-Nuclear Magnetic Resonance (CMP-NMR) probe allows detailed study of all phases within unaltered natural samples. This technology enables analysis of structures and interactions across liquid, gel, and solid components in situ.

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Metabolomic Analysis of Rat Brain by High Resolution Nuclear Magnetic Resonance Spectroscopy of Tissue Extracts
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Metabolomic Analysis of Rat Brain by High Resolution Nuclear Magnetic Resonance Spectroscopy of Tissue Extracts

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Metabolomic Analysis of Rat Brain by High Resolution Nuclear Magnetic Resonance Spectroscopy of Tissue Extracts
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Metabolomic Analysis of Rat Brain by High Resolution Nuclear Magnetic Resonance Spectroscopy of Tissue Extracts

Published on: September 21, 2014

Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Biophysics

Background:

  • Heterogeneous samples (soils, tissues, etc.) possess complex environmental and biological properties determined by the interplay of liquid, gel, and solid phases.
  • Studying individual phases separately risks altering the sample and losing crucial interfacial and conformational information.
  • Existing NMR techniques often struggle to analyze all phases simultaneously within an intact sample.

Purpose of the Study:

  • To introduce a novel Comprehensive Multiphase-Nuclear Magnetic Resonance (CMP-NMR) probe designed for analyzing heterogeneous samples.
  • To enable the study of all chemical bonds within all phases of unaltered natural samples.
  • To investigate structures and interactions within and between different phases of heterogeneous samples.

Main Methods:

  • Development and implementation of a Comprehensive Multiphase-Nuclear Magnetic Resonance (CMP-NMR) probe.
  • The probe incorporates high power circuitry, Magic Angle Spinning (MAS), a lock channel, pulse field gradients, and susceptibility matching.
  • Experimental validation using a model multiphase sample and soil samples with contaminants, analyzing (1)H, (13)C, and (19)F spectra.

Main Results:

  • The CMP-NMR probe successfully differentiated and studied components in liquid, gel, and solid phases of a model heterogeneous sample, yielding separate (1)H and (13)C spectra.
  • (19)F NMR demonstrated capability in analyzing soil samples with contaminants, showcasing a practical application.
  • The technology allows for independent study of structures and interactions within each phase, as well as transfers between phases.

Conclusions:

  • The developed CMP-NMR probe overcomes limitations of traditional methods by allowing in situ analysis of all phases in natural, unaltered heterogeneous samples.
  • This novel NMR approach offers significant potential for studying the complex interplay of components in diverse natural systems.
  • The probe facilitates a deeper understanding of chemical interactions and kinetics at interfaces within complex sample matrices.