General Guidelines for Sample Preparation Strategies in HR-$\mu$MAS NMR-based Metabolomics of Microscopic Specimens

Covadonga Lucas-Torres (1) , Thierry Bernard (2) , Gaspard Huber (1) , Patrick Berthault (1) , Yusuke Nishiyama (3) , Pancham S. Kandiyal (4) , Bénédicte Elena-Herrmann (4) , Laurent Molin (5) , Florence Solari (5) , Anne-Karine Bouzier-Sore (6) , Alan Wong (1)

1 LSDRM - Laboratoire Structure et Dynamique par Résonance Magnétique (LCF)
2 NIMBE UMR 3685 - Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M)
3 JEOL
4 IAB - Institute for Advanced Biosciences / Institut pour l'Avancée des Biosciences (Grenoble)
5 UCBL - Université Claude Bernard Lyon 1
6 CRMSB - Centre de résonance magnétique des systèmes biologiques

The study of the metabolome within tissues, organisms, cells or biofluids can be carried out by several bioanalytical techniques. Among them, nuclear magnetic resonance (NMR) is one of the principal spectroscopic methods. This is due to a sample rotation technique, high-resolution magic angle spinning (HR-MAS), which targets the analysis of heterogeneous specimens with a bulk sample mass from 5 to 10 mg. Recently, a new approach, high-resolution micro-magic angle spinning (HR-$\mu$MAS), has been introduced. It opens, for the first time, the possibility of investigating microscopic specimens (<500 $\mu$g) with NMR spectroscopy, strengthening the concept of homogeneous sampling in a heterogeneous specimen. As in all bioanalytical approaches, a clean and reliable sample preparation strategy is a significant component in designing metabolomics (oromics, in general) studies. The sample preparation for HR-$\mu$MAS is consequentially complicated by the $\mu$g-scale specimen and has yet to be addressed. This report details the strategies for three specimen types: biofluids, fluid matrices and tissues. It also provides the basis for designing future μMAS NMR studies of microscopic specimens.

Keywords: NMR; microscopic samples; metabolomics; sample preparation; high-resolution magic angle spinning

Domains: Material chemistry; Theoretical and/or physical chemistry

Covadonga Lucas-Torres, Thierry Bernard, Gaspard Huber, Patrick Berthault, Yusuke Nishiyama, et al.. General Guidelines for Sample Preparation Strategies in HR-$\mu$MAS NMR-based Metabolomics of Microscopic Specimens. Metabolites, 2020, 10 (2), pp.54. ⟨10.3390/metabo10020054⟩. ⟨cea-02464528⟩