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Related Concept Videos

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

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At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
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The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
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Other Nuclides: 31P, 19F, 15N NMR01:16

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Many organic, inorganic, and biological molecules contain spin-half nuclei such as nitrogen-15, fluorine-19, and phosphorus-31. As a result, NMR studies of these nuclei have found extensive applications in chemical and biological research.
While fluorine-19 and phosphorous-31 have high natural abundances (100%) and positive gyromagnetic ratios, nitrogen-15 has a low natural abundance and a negative gyromagnetic ratio. However, nitrogen-15 is still preferred over nitrogen-14 (which has a...
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Phospholipids in Motion: High-Resolution 31P NMR Field Cycling Studies.

Mary F Roberts1, Jingfei Cai1, Sivanandam V Natarajan2

  • 1Department of Chemistry, Boston College, Chestnut Hill, Massachusetts 02467, United States.

The Journal of Physical Chemistry. B
|July 29, 2021
PubMed
Summary
This summary is machine-generated.

High-resolution 31P NMR spin-lattice relaxometry quantifies diverse phospholipid motions. This technique reveals lipid dynamics and structure, offering insights into membrane function and additive effects.

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Area of Science:

  • Biophysics
  • Membrane biophysics
  • Nuclear Magnetic Resonance (NMR) spectroscopy

Background:

  • Phospholipid dynamics are crucial for membrane function but challenging to quantify.
  • Nuclear Magnetic Resonance (NMR) relaxation provides insights into molecular motion and structure.

Purpose of the Study:

  • To develop and apply high-resolution field cycling 31P NMR spin-lattice relaxometry for detailed analysis of phospholipid dynamics.
  • To quantify various phospholipid motions, including lateral diffusion and rotational dynamics, within membrane structures.
  • To assess the impact of additives on phospholipid behavior and molecular dynamics.

Main Methods:

  • Utilized high-resolution field cycling 31P NMR spin-lattice relaxometry.
  • Measured the field dependence of the 31P spin-lattice relaxation rate (R1) across a wide magnetic field range (11.74 to 0.003 T).
  • Analyzed nuclear magnetic relaxation dispersions (NMRDs) and chemical shift anisotropy contributions to R1.

Main Results:

  • Identified three dipolar NMRDs and one from 31P chemical shift anisotropy contributing to R1.
  • Extracted correlation times and relaxation amplitudes to determine lateral diffusion constants and rotational motion parameters.
  • Revealed that polar headgroup motion is not restricted on a microsecond timescale and quantified average 31P-1H angles.

Conclusions:

  • Field cycling 31P NMR relaxometry is a powerful technique for dissecting complex phospholipid dynamics in various membrane mimetics.
  • The method allows for the quantification of lipid diffusion, rotational motion, and the effects of additives on these dynamics.
  • This approach is versatile for studying lipid behavior in small unilamellar vesicles, micelles, and nanodisks.