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Related Experiment Video

Updated: Jul 10, 2026

Single Molecule Analysis of Laser Localized Psoralen Adducts

Single Molecule Analysis of Laser Localized Psoralen Adducts

Published on: April 20, 2017

Proton-detected separated local field spectroscopy.

Chin H Wu¹, Stanley J Opella

¹Department of Chemistry and Biochemistry, 9500 Gilman Drive, University of California, San Diego, La Jolla, CA 92093-0307, USA.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)

|November 6, 2007

Summary

This study demonstrates PISEMO, a nuclear magnetic resonance (NMR) technique for analyzing peptides. Proton (1H) detection offers a significantly improved signal-to-noise ratio compared to nitrogen (15N) detection.

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Area of Science:

* Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
* Biophysical Chemistry
* Structural Biology

Background:

* Nuclear Magnetic Resonance (NMR) is crucial for determining molecular structures.
* Solid-state NMR experiments often face challenges with signal-to-noise ratios and resolution.
* Separated local field experiments aim to enhance spectral information in solid samples.

Purpose of the Study:

* To demonstrate the application of the PISEMO (Phase-Insensitive Spin Echo Multiple Acquisition) experiment.
* To evaluate the performance of PISEMO using direct nitrogen-15 (15N) or carbon-13 (13C) detection versus indirect proton (1H) detection.
* To assess spectral resolution and signal-to-noise ratios for peptide structural analysis.

Main Methods:

* Implementation of the PISEMO experiment on a single crystal of a model peptide.
* Utilizing multiple-pulse sequences to suppress proton-proton (1H-1H) homonuclear couplings.
* Observing proton (1H) signals modulated by proton-nitrogen (1H-15N) heteronuclear couplings stroboscopically.
* Comparing spectra obtained with direct 15N detection and indirect 1H detection.

Main Results:

* Proton (1H) detection in PISEMO yielded spectra with approximately 2.5 times higher signal-to-noise ratio compared to 15N detection.
* Spectral resolution in both the 15N chemical shift and 1H-15N heteronuclear coupling dimensions was comparable to existing PISEMA methods.
* The use of on-resonance pulses improved spectral bandwidth.

Conclusions:

* Proton (1H) detection significantly enhances sensitivity in PISEMO experiments for solid-state NMR.
* PISEMO provides a valuable tool for high-resolution structural studies of peptides and other biomolecules.
* The improved signal-to-noise ratio facilitates more efficient structural elucidation using solid-state NMR.