Related Experiment Video
Updated: Jan 30, 2026
08:54
NMR Spectroscopy as a Robust Tool for the Rapid Evaluation of the Lipid Profile of Fish Oil Supplements
Published on: May 1, 2017
26.8K
Analytical Evaluation of Low-Field 31P NMR Spectroscopy for Lipid Analysis
Boris Gouilleux1, Nichlas Vous Christensen1, Kirsten G Malmos1
1Interdisciplinary Nanoscience Center and Department of Chemistry , Aarhus University , Gustav Wieds Vej 14 , DK-8000 Aarhus C, Denmark.
Analytical Chemistry
|January 19, 2019
Summary
Simple 31P NMR using benchtop spectrometers can detect and identify phospholipids in complex mixtures. This technique offers new opportunities for routine analyses in food and health sciences.
Area of Science:
- Analytical Chemistry
- Biochemistry
- Spectroscopy
Background:
- Phosphorus-31 Nuclear Magnetic Resonance (31P NMR) is crucial for lipidomics in food and health sciences.
- Compact, maintenance-free benchtop NMR spectrometers are advancing routine analyses.
Purpose of the Study:
- To evaluate the analytical performance of 31P NMR using benchtop spectrometers for phospholipid analysis.
- To assess the detection, identification, and quantification capabilities for phospholipids in complex mixtures.
Main Methods:
- Utilizing heteronuclear cross-polarization experiments for phospholipid detection.
- Employing 2D 1H-31P total correlated spectroscopy (TOCSY) for headgroup assignment.
- Developing and evaluating two quantitative methods for absolute concentration determination.
Main Results:
- Phospholipids detected within 2 hours with limits of detection as low as 0.5 mM (1 T) and 0.2 mM (2 T).
- Unambiguous assignment of phosphatidylcholine (PC), phosphatidylethanolamine (PE), phosphatidylinositol (PI), phosphatidylserine (PS), and phosphatidylglycerol (PG) headgroups.
- Evaluation of precision and accuracy for proposed quantitative methods.
Conclusions:
- Benchtop 31P NMR is a viable technique for analyzing phospholipids in complex mixtures.
- The method enables sensitive detection, identification, and quantification, advancing lipidomics applications.
- Improvements in compact NMR technology open new avenues for routine analysis in various scientific fields.
![Investigating Cardiac Metabolism in the Isolated Perfused Mouse Heart with Hyperpolarized [1-13C]Pyruvate and 13C/31P NMR Spectroscopy](/_next/image?url=https%3A%2F%2Fcloudfront.jove.com%2FCDNSource%2Fteasers%2F63188.jpg&w=3840&q=50)
Related Concept Videos
01:19NMR Spectroscopy Of Amines
11.1K
In proton NMR spectroscopy, primary amines and secondary amines showcase their N–H protons as a broad signal in the chemical shift range between δ 0.5 and 5 ppm. The exact position in this range depends on several factors, including sample concentration, hydrogen bonding, and the type of solvent used. Since amine protons undergo fast proton exchange in solution, the protons are labile and therefore do not participate in any splitting with adjacent protons. Thus, the observed peak is...
11.1K
01:14NMR Spectroscopy of Aromatic Compounds
6.3K
Aromatic compounds can be identified or analyzed using proton NMR and carbon‐13 NMR. Typically, aromatic hydrogens or hydrogens directly bonded to the aromatic rings are strongly deshielded by the aromatic ring current. Therefore, they absorb in the range of 6.5–8.0 ppm in proton NMR spectra. For instance, aromatic hydrogens directly bonded to the benzene ring absorb at 7.3 ppm. However, aromatic hydrogens of larger rings absorb farther upfield or downfield than the ideal range.
6.3K
01:34NMR Spectroscopy of Benzene Derivatives
11.1K
Simple unsubstituted benzene has six aromatic protons, all chemically equivalent. Therefore, benzene exhibits only a singlet peak at δ 7.3 ppm in the 1H NMR spectrum. The observed shift is far downfield because the aromatic ring current strongly deshields the protons. Any substitution on the benzene ring makes the aromatic protons nonequivalent, and the protons split each other. The peak is, therefore, no longer a singlet and the splitting pattern and their associated coupling...
11.1K
01:15NMR Spectroscopy: Chemical Shift Overview
3.3K
The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
For instance, the proton...
3.3K
01:08NMR Spectroscopy: Spin–Spin Coupling
3.2K
The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved...
3.2K
01:30NMR and Mass Spectroscopy of Carboxylic Acids
5.3K
In ¹H NMR spectroscopy, acidic protons (–COOH) of carboxylic acids are highly deshielded and absorb far downfield, at around 9–12 ppm. The chemical shift value depends on the concentration and solvent used.
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the...
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the...
5.3K