HAL will be down for maintenance from Friday, June 10 at 4pm through Monday, June 13 at 9am. More information
Skip to Main content Skip to Navigation
Journal articles

High resolution magic angle spinning NMR to investigate ligand-receptor binding events for mass-limited samples in liquids

Abstract : This work shows that high resolution magic angle spinning (HR-MAS) can be used to elucidate ligand receptor binding phenomena for mass-limited samples in liquid solution. With respect to conventional 5 mm liquid-state NMR probe heads, HR-MAS allows for a considerable reduction (about one order of magnitude) in sample volume requirement, which represents a considerable advantage when working with biological samples present in low amount. More specifically, using a 20-mu L. active volume HR-MAS probe head, NMR experiments typically used to describe binding events (e.g. Saturation Transfer Difference, WaterLOGSY, Diffusion Ordered Spectroscopy) were successfully recorded. In fact, contrary to other NMR experiments (e.g. TOCSY), which require special care when performed on liquid samples by HR-MAS, no interferences due to fast sample spinning were observed here. Collectively, the results indicate that HR-MAS allows for a significant mass sensitivity enhancement (a 3-fold increase in signal-to-noise ratio per unit of measuring time and mass was obtained here), hereby improving correspondingly the detection limit of the previously mentioned NMR experiments. More importantly, because MAS removes magnetic susceptibility broadenings in the sample, a good spectral resolution can be easily achieved in HR-MAS even for slightly heterogeneous samples, such as those arising from incomplete purification. (C) 2011 Elsevier B.V. All rights reserved.
Document type :
Journal articles
Complete list of metadata

Contributor : Didier Gigmes Connect in order to contact the contributor
Submitted on : Tuesday, February 7, 2017 - 4:42:22 PM
Last modification on : Tuesday, December 14, 2021 - 8:42:07 AM




Fabio Ziarelli, Ling Peng, Cheng-Cai Zhang, Stéphane Viel. High resolution magic angle spinning NMR to investigate ligand-receptor binding events for mass-limited samples in liquids. Journal of Pharmaceutical and Biomedical Analysis, Elsevier, 2012, 59, pp.13--17. ⟨10.1016/j.jpba.2011.10.006⟩. ⟨hal-01460455⟩



Record views