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Related Concept Videos

¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.2K
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...
1.2K
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

2.5K
The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
2.5K
¹H NMR Signal Integration: Overview00:58

¹H NMR Signal Integration: Overview

2.7K
The intensity of a signal, which can be represented by the area under the peak, depends on the number of protons contributing to that signal. The area under each peak is shown as a vertical line called an integral, with the integral value listed under it, as seen in the proton NMR spectrum of benzyl acetate. Each integral value is divided by the smallest integral value to obtain the ratio of the number of protons producing each signal. The ratio reveals the relative number of protons and not...
2.7K
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

1.4K
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...
1.4K
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

1.0K
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....
1.0K
NMR Spectroscopy of Aromatic Compounds01:14

NMR Spectroscopy of Aromatic Compounds

5.3K
Aromatic compounds can be identified or analyzed using proton NMR and carbon‐13 NMR. Typically, aromatic hydrogens or hydrogens directly bonded to the aromatic rings are strongly deshielded by the aromatic ring current. Therefore, they absorb in the range of 6.5–8.0 ppm in proton NMR spectra. For instance, aromatic hydrogens directly bonded to the benzene ring absorb at 7.3 ppm. However, aromatic hydrogens of larger rings absorb farther upfield or downfield than the ideal range.
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Concentration of Metabolites from Low-density Planktonic Communities for Environmental Metabolomics using Nuclear Magnetic Resonance Spectroscopy
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NMR for Mixture Analysis: Concentration-Ordered Spectroscopy.

Bin Yuan1,2, Zhiming Zhou1,2, Bin Jiang1,2

  • 1State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, National Center for Magnetic Resonance in Wuhan, Wuhan Institute of Physics and Mathematics, Innovation Academy for Precision Measurement Science and Technology, Chinese Academy of Sciences-Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan 430071, China.

Analytical Chemistry
|July 6, 2021
PubMed
Summary
This summary is machine-generated.

Concentration-ordered NMR spectroscopy (CORDY) quantifies compounds in complex mixtures by relating NMR peak area to concentration. This novel method, CORDY, successfully separates and quantifies components in diverse samples.

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy

Background:

  • Nuclear Magnetic Resonance (NMR) spectroscopy is crucial for chemical analysis.
  • Quantifying components in complex mixtures using NMR presents significant challenges.

Purpose of the Study:

  • To introduce a novel NMR approach, concentration-ordered NMR spectroscopy (CORDY).
  • To enable simultaneous separation and quantification of components in complex samples.

Main Methods:

  • CORDY utilizes the proportionality between NMR peak area, spin number, and compound concentration.
  • It incorporates prior chemical shift and line shape information to refine analysis.
  • Generates a pseudo-2D spectrum with chemical shifts and concentrations.

Main Results:

  • CORDY successfully separated and quantified components in a model amino acid mixture, Red Bull, and human urine.
  • The method achieved separation across two orders of magnitude in concentration.
  • Combining CORDY with DOSY (CORDY-DOSY) enhanced resolution for molecules with similar concentrations or diffusion coefficients.

Conclusions:

  • CORDY offers a powerful new tool for quantitative analysis of complex mixtures using NMR.
  • The CORDY-DOSY combination provides improved resolution for challenging samples.