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

Nghia Tuan Tuan Duong (1) , Masanori Yamato (2, 3) , Masayuki Nakano (4, 3) , Satoshi Kume (2, 3) , Yasuhisa Tamura (2, 3) , Yosky Kataoka (2, 3, 4) , Alan Wong (5) , Yusuke Nishiyama (6, 1)

1 RIKEN CLST-JEOL - Advanced Solid-State NMR Unit
2 RIKEN CLST-JEOL - Multi-Modal Microstructure Analysis Unit
3 RIKEN CLST - RIKEN Center for Life Science Technologies
4 Osaka City University Graduate Medical School
5 LSDRM - Laboratoire Structure et Dynamique par Résonance Magnétique (LCF)
6 JEOL Ltd, 1156 Nakagami, Akishima, Tokyo 196-0022, Japan.

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.

Keywords: NMR; metabolomics; metabolites; HRµMAS; capillary-inserted rotor; mass-limited neurospheres

Domains: Material chemistry

Nghia Tuan Tuan Duong, Masanori Yamato, Masayuki Nakano, Satoshi Kume, Yasuhisa Tamura, et al.. Capillary-Inserted Rotor Design for HRµMAS NMR-Based Metabolomics on Mass-Limited Neurospheres. Molecules, 2017, 22 (8), pp.1289. ⟨10.3390/molecules22081289⟩. ⟨cea-01573213⟩