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Molecules 2017, 22(8), 1289;

Capillary-Inserted Rotor Design for HRµMAS NMR-Based Metabolomics on Mass-Limited Neurospheres

Advanced Solid-State NMR Unit, RIKEN CLST-JEOL Collaboration Center, RIKEN, Yokohama, Kanagawa 230-0045, Japan
Multi-Modal Microstructure Analysis Unit, RIKEN CLST-JEOL Collaboration Center, RIKEN, Kobe, Hyogo 650-0047, Japan
Cellular Function Imaging Team, RIKEN Center for Life Science Technologies, Kobe, Hyogo 650-0047, Japan
Department of Physiology, Osaka City University Graduate School of Medicine, Abeno-ku, Osaka 545-8585, Japan
NIMBE, CEA, CNRS, Université Paris-Saclay, CEA Saclay, 91191 Gif-sur-Yvette, France
Engineering Division, JEOL RESONANCE Inc., Musashino, Akishima, Tokyo 196-8558, Japan
Author to whom correspondence should be addressed.
Received: 24 June 2017 / Accepted: 30 July 2017 / Published: 3 August 2017
(This article belongs to the Special Issue Recent Advances in Biomolecular NMR Spectroscopy)
Full-Text   |   PDF [698 KB, uploaded 8 August 2017]   |  


Nuclear magnetic resonance (NMR) spectroscopy is a powerful analytical technique and has been widely used in metabolomics. However, the intrinsic low sensitivity of NMR prevents its applications to systems with limited sample availabilities. In this study, a new experimental approach is presented to analyze mass-scarce samples in limited volumes of less than 300 nL with simple handling. The sample is loaded into the glass capillary, and this capillary is then inserted into a Kel-F rotor. The experimental performance of the capillary-inserted rotor (capillary-insert) is investigated on an isotropic solution of sucrose by the use of a high-resolution micro-sized magic angle spinning (HRµMAS) probe. The acquired NMR signal’s sensitivity to a given sample amount is comparable or even higher in comparison to that recorded by the standard solution NMR probe. More importantly, this capillary-insert coupled with the HRµMAS probe allows in-depth studies of heterogeneous samples as the MAS removes the line broadening caused by the heterogeneity. The NMR analyses of mass-limited cultured neurospheres have been demonstrated, resulting in high quality spectra where numerous metabolites are unambiguously identified. View Full-Text
Keywords: NMR; metabolomics; metabolites; HRµMAS; capillary-inserted rotor; mass-limited neurospheres NMR; metabolomics; metabolites; HRµMAS; capillary-inserted rotor; mass-limited neurospheres

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Duong, N.T.; Yamato, M.; Nakano, M.; Kume, S.; Tamura, Y.; Kataoka, Y.; Wong, A.; Nishiyama, Y. Capillary-Inserted Rotor Design for HRµMAS NMR-Based Metabolomics on Mass-Limited Neurospheres. Molecules 2017, 22, 1289.

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