Chemical Physics Letters, Vol.485, No.4-6, 275-280, 2010
Proton micro-magic-angle-spinning NMR spectroscopy of nanoliter samples
We present our recent progress in the development of micro-magic-angle-spinning solenoid-based probeheads for the application in high-resolution H-1 solid-state NMR of nanoliter sample volumes. The use of fused-silica capillaries as sample holders results in spectra without any 1H background signal. It is possible to obtain H-1 spectra of 40-80 nl samples in a few scans. We obtained high-resolution H-1 spectra employing different homonuclear decoupling sequences on powdered samples of L-alanine, the tripeptide AGG, and a single crystal of L-tyrosine center dot HCl. In addition, we recorded high-resolution two-dimensional proton-detected H-1-C-13 heteronuclear correlation spectra of [U-C-13(3), N-15]-L-alanine and AGG with natural abundant isotope distribution. Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.