Proton Micro-Magic-Angle-Spinning NMR Spectroscopy of Nanoliter Samples ,

A. Brinkmann*, S. K. Vasa, H. Janssen, A. P. M. Kentgens,
Chem. Phys. Lett. 485, 275-280, (2010).
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We present our recent progress in the development of micro-​magic-​angle-​spinning solenoid-​based probeheads for the application in high-​resolution 1H 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 1H spectra of 40–80 nl samples in a few scans. We obtained high-​resolution 1H spectra employing different homonuclear decoupling sequences on powdered samples of L-alanine, the tripeptide AGG, and a single crystal of L-tyrosine · HCl. In addition, we recorded high-​resolution two-​dimensional proton-​detected 1H–13C heteronuclear correlation spectra of [U-13C3,15N]-L-alanine and AGG with natural abundant isotope distribution.