Open AccessAnalytical Evaluation of Low-Field 31P NMR Spectroscopy for Lipid Analysis
Author(s) -
Boris Gouilleux,
Nichlas Vous Christensen,
Kirsten Gade Malmos,
Thomas Vosegaard
Publication year - 2019
Publication title -
analytical chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 2.117
H-Index - 332
eISSN - 1520-6882
pISSN - 0003-2700
DOI - 10.1021/acs.analchem.8b05416
Subject(s) - chemistry , analytical chemistry (journal) , spectrometer , nuclear magnetic resonance spectroscopy , lipidomics , analyser , heteronuclear molecule , phosphatidylcholine , nmr spectra database , detection limit , spectroscopy , chromatography , phospholipid , spectral line , membrane , organic chemistry , biochemistry , physics , quantum mechanics , astronomy
We investigate the potential of 31 P NMR with simple, maintenance-free benchtop spectrometers to probe phospholipids in complex mixtures. 31 P 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 new opportunities for NMR routine analyses. A prior milestone is the evaluation of the analytical performance provided by 31 P 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 phosphatidylcholine (PC), phosphatidyl-ethanolamine (PE), phosphatidylinositol (PI), phosphatidylserine (PS), and phosphatidyl-glycerol (PG) can be unambiguously assigned based on 2D 1 H- 31 P total correlated spectroscopy (TOCSY) spectra. Furthermore, two quantitative methods to obtain absolute concentrations are proposed and discussed, and the performance is evaluated regarding precision and accuracy.