JEOL : Novel Three-Dimensional Correlation Experiments to Reveal Local Proton Networks under Fast Magic-Angle Spinning at Natural 13C Abundance
October 18, 2017 at 08:26 pm EDT
Share
H double quantum (DQ)/H single quantum (SQ) correlation solid-state NMR spectroscopy is widely used to obtain internuclear H-H proximities, especially at fast magic angle spinning (MAS) rate > 60 kHz. However, H signals are not well-resolved due to intense H-H homonuclear dipolar interactions even at the attainable maximum MAS frequencies of ~100 kHz to date. We have recently introduced novel three-dimensional (3D) experiments to resolve the H DQ/H SQ correlation peaks using the additional C dimension. Although the low natural abundance of C (1.1%) significantly reduces the sensitivities, the H indirect measurements alleviate this issue and make this experiment possible. The two different implementations of C/H DQ/H SQ correlations and H DQ/C/H SQ correlations have been discussed and demonstrated using L-histidine.HCl.HO at natural abundance to reveal the local H-H networks nearby each C. In addition, the complete H resonance assignments have been achieved from a single 3D C/H DQ/H SQ experiment. We have also demonstrated the applicability of our proposed method on a biologically relevant molecule capsaicin.
The 2D H DQ/H SQ spectrum of capsaicin (left) is too complex due to signal overlaps. On the other hand, the C-filtered spectrum (right) yields well-resolved peaks and thus signal assignment is possible. Both spectra were recorded at 70 kHz MAS. Please refer to the original paper for more detail.
M. Malon, M. K. Pandey and Y. Nishiyama, J. Phys. Chem. B, 2017, 121, 8123-8131.
If you want to see a printed version,
please click this PDF file.PDF 266KB
Jeol Ltd. published this content on 19 October 2017 and is solely responsible for the information contained herein. Distributed by Public, unedited and unaltered, on 19 October 2017 00:25:02 UTC.
Original documenthttps://www.jeol.co.jp/en/applications/detail/1521.html
Public permalinkhttp://www.publicnow.com/view/C2BE13358C629E8F4CAA25462CC46D9F14E08D31
JEOL Ltd. is a Japan-based company mainly engaged in the manufacture, sale, maintenance, development and research of scientific instruments, semiconductor related equipment, industrial and medical equipment, and related products and parts. It operates through three business segments. Science and Measurement Equipment segment manufactures and sells three types of equipment. Electron optical devices include electron microscopes, peripheral devices and others. Analytical instruments include nuclear magnetic resonance equipment, electron spin resonance equipment and others. Measurement and inspection equipment include scanning electron microscopes, analytical scanning electron microscopes, peripheral equipment and others. Industrial Equipment segment manufactures and sells electron beam lithography equipment, linear electron guns and power supplies and others. Medical Equipment segment manufactures and sells clinical test information processing systems, and automatic amino acid analyzers.