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 (1)H 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 (1)H spectra of 40-80 nl samples in a few scans. We obtained high-resolution (1)H 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 (1)H-(13)C heteronuclear correlation spectra of [U-(13)C(3), (15)N]-L-alanine and AGG with natural abundant isotope distribution. Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.