Analytical Evaluation of Low-Field 31P NMR Spectroscopy for Lipid Analysis

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Abstract
We investigate the potential of 31P NMR with simple, maintenance-free benchtop spectrometers to probe phospholipids in complex mixtures. 31P NMR-based lipidomics has become an important topic in a wide range of applications in food- and health-sciences, and the continuous improvements of compact, maintenance- and cryogen-free instruments opens news opportunities for NMR routine analyses. A prior milestone is the evaluation of the analytical performance provided by 31P NMR at low magnetic field. To address this, we assess the ability of state-of-the-art benchtop NMR spectrometers to detect, identify and quantify several types of phospholipids in mixtures. Relying on heteronuclear cross-polarization experiments, phospholipids can be detected in 2 h with a limit of detection of 0.5 mM at 1 T and 0.2 mM at 2 T, while the headgroups of PC, PE, PI, PS and PG can be unambiguously assigned based on 2D 1H-31P TOCSY spectra. Furthermore, two quantitative methods to obtain absolute concentrations are proposed and discussed, and the performance is evaluated regarding precision and accuracy.
Funding Information
  • Novo Nordisk (NNF16OC0021110)
  • Uddannelses- og Forskningsministeriet (AU-2010-612-181)
  • H2020 Future and Emerging Technologies (731475)
  • H2020 Research Infrastructures (731005)
  • Carlsbergfondet (CF15-211)

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