Highly Repeatable Dissolution Dynamic Nuclear Polarization for Heteronuclear NMR Metabolomics

Anal Chem. 2016 Jun 21;88(12):6179-83. doi: 10.1021/acs.analchem.6b01094. Epub 2016 Jun 13.

Abstract

At natural (13)C abundance, metabolomics based on heteronuclear NMR is limited by sensitivity. We have recently demonstrated how hyperpolarization by dissolution dynamic nuclear polarization (D-DNP) assisted by cross-polarization (CP) provides a reliable way of enhancing the sensitivity of heteronuclear NMR in dilute mixtures of metabolites. In this Technical Note, we evaluate the precision of this experimental approach, a critical point for applications to metabolomics. The higher the repeatability, the greater the likelihood that one can detect small biologically relevant differences between samples. The average repeatability of our state-of-the-art D-DNP NMR equipment for samples of metabolomic relevance (20 mg dry weight tomato extracts) is 3.6% for signals above the limit of quantification (LOQ) and 6.4% when all the signals above the limit of detection (LOD) are taken into account. This first report on the repeatability of D-DNP highlights the compatibility of the technique with the requirements of metabolomics and confirms its potential as an analytical tool for such applications.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Carbon Isotopes / chemistry
  • Fruit / metabolism
  • Limit of Detection
  • Metabolomics / methods*
  • Nuclear Magnetic Resonance, Biomolecular*
  • Reproducibility of Results
  • Signal-To-Noise Ratio
  • Solanum lycopersicum / growth & development
  • Solanum lycopersicum / metabolism

Substances

  • Carbon Isotopes
  • Carbon-13