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

NMR Spectroscopy: Chemical Shift Overview

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...
Proton (¹H) NMR: Chemical Shift01:07

Proton (¹H) NMR: Chemical Shift

Organic molecules primarily contain carbon and hydrogen atoms. While all the hydrogen isotopes are NMR-active, protium or hydrogen-1 is the most abundant. It has a significant energy separation between its nuclear spin states due to its large gyromagnetic ratio. As per Boltzmann's distribution, an increase in the energy separation implies a greater excess population of nuclei available for excitation, resulting in a strong NMR absorption signal.
Absorption signals of all the protium nuclei in a...

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Pure Shift Nuclear Magnetic Resonance: a New Tool for Plant Metabolomics
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Chemical shift correlations from hyperpolarized NMR using a single SHOT.

Guannan Zhang1, Franz Schilling, Steffen J Glaser

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

Analytical Chemistry
|January 29, 2013
PubMed
Summary

This study introduces a new NMR method, scaling of heteronuclear couplings by optimal tracking (SHOT), to overcome signal loss in hyperpolarized molecules. SHOT enables rapid chemical shift correlation analysis from a single spectrum, enhancing molecular characterization.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Physical Chemistry
  • Spectroscopic Techniques

Background:

  • Dynamic nuclear polarization (DNP) enhances NMR signals but hyperpolarized states are non-renewable.
  • This limitation prevents traditional 2D correlation spectroscopy, crucial for molecular structure determination.
  • Novel methods are needed to circumvent this issue for DNP-enhanced NMR.

Purpose of the Study:

  • To introduce and validate the scaling of heteronuclear couplings by optimal tracking (SHOT) method.
  • To enable chemical shift correlation analysis in DNP-enhanced NMR despite non-renewable polarization.
  • To demonstrate a simplified and accurate approach for molecular structural characterization.

Main Methods:

  • Application of SHOT decoupling pulses optimized via optimal control algorithms.
  • Acquisition of single 1D (13)C or (1)H spectra with off-resonance decoupling.
  • Testing the method on vanillin, a molecule with diverse functional groups.
  • Optimization strategies included linear and alternating linear responses to chemical shift offset.

Main Results:

  • Successful acquisition of chemical shift correlations in C-H groups from single spectra.
  • Demonstrated SHOT decoupling for simplified and accurate data analysis on vanillin.
  • Achieved high accuracy with error ranges of ±0.03 ppm for (1)H and ±0.4 ppm for (13)C shifts.
  • Maximized signal-to-noise ratio by obtaining correlations from a single scan.

Conclusions:

  • SHOT provides a viable solution for chemical shift correlation in DNP-enhanced NMR.
  • The method allows for rapid acquisition and controlled accuracy of spectral data.
  • SHOT offers potential for real-time spectroscopy applications due to its speed and efficiency.