Very fast magic angle spinning (1)H-(14)N 2D solid-state NMR: sub-micro-liter sample data collection in a few minutes

J Magn Reson. 2011 Jan;208(1):44-8. doi: 10.1016/j.jmr.2010.10.001. Epub 2010 Oct 8.

Abstract

Substantial resolution and sensitivity enhancements of solid-state (1)H detected (14)N HMQC NMR spectra at very fast MAS rates up to 80 kHz, in a 1mm MAS rotor, are presented. Very fast MAS enhances the (1)H transverse relaxation time and efficiently decouples the (1)H-(14)N interactions, both effects leading to resolution enhancement. The micro-coil contributes to the sensitivity increase via strong (14)N rf fields and high sensitivity per unit volume. (1)H-(14)N HMQC 2D spectra of glycine and glycyl-L-alanine at 70 kHz MAS at 11.7 T are observed in a few minutes with a sample volume of 0.8 μL.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Alanine / analysis*
  • Glycine / analysis*
  • Magnetic Resonance Spectroscopy / methods*
  • Microchemistry / methods*
  • Nitrogen / analysis*
  • Protons
  • Spin Labels

Substances

  • Protons
  • Spin Labels
  • Nitrogen
  • Alanine
  • Glycine