A multidimensional 1H NMR lipidomics workflow to address chemical food safety issues
Although it is still at a very early stage compared to its mass spectrometry (MS) counterpart, proton nuclear magnetic resonance (NMR) lipidomics is worth being investigated as an original and complementary solution for lipidomics. Dedicated sample preparation protocols and adapted data acquisition methods have to be developed to set up an NMR lipidomics workflow; in particular, the considerable overlap observed for lipid signals on 1D spectra may hamper its applicability.
The study describes the development of a complete proton NMR lipidomics workflow for application to serum fingerprinting. It includes the assessment of fast 2D NMR strategies, which, besides reducing signal overlap by spreading the signals along a second dimension, offer compatibility with the high-throughput requirements of food quality characterization.
The robustness of the developed sample preparation protocol is assessed in terms of repeatability and ability to provide informative fingerprints; further, different NMR acquisition schemes—including classical 1D, fast 2D based on non-uniform sampling or ultrafast schemes—are evaluated and compared. Finally, as a proof of concept, the developed workflow is applied to characterize lipid profiles disruption in serum from β-agonists diet fed pigs.
Our results show the ability of the workflow to discriminate efficiently sample groups based on their lipidic profile, while using fast 2D NMR methods in an automated acquisition framework.
This work demonstrates the potential of fast multidimensional 1H NMR—suited with an appropriate sample preparation—for lipidomics fingerprinting as well as its applicability to address chemical food safety issues.
KeywordsLipidomics NMR fingerprinting Ultrafast NMR Non uniform sampling Serum Food quality
The authors would like to thank the Région Pays de la Loire for funding through the “Recherche-Formation-Innovation: Food 4.2” program (Grant LipidoTool) and the technical platform CORSAIRE.
GDP, BLB and PG designed research; JM performed research; EM contributed analytic tools; JM, EM, YG, GDP and PG analyzed data; JM, PG and GDP wrote the paper. All authors read and approved the manuscript.
Compliance with ethical standards
Conflict of interest
The authors declare that they have no conflict of interest.
Research Involving Animal Participants
The animal study was approved by the national Ethical Committee n°6 (Comité n°6 - Ministère de l’Enseignement Supérieur et de la Recherche – Direction Générale pour la Recherche et l’Innovation – Secrétariat « Autorisation de projet » - 1, rue Descartes, 75231 PARIS cedex 5) under agreement 2,015,092,516,084,715/APAFIS 1914 (Protocol Number CRIP-2015-054). The study was implemented at Centre de Recherche et d’Investigation Préclinique-CRIP-ONIRIS- Plate-forme de chirurgie et animaleries expérimentales, Oniris, Nantes, France, under agreement number F.44-271.
Institutional and national guidelines were followed for the animal experimentation, as mentioned in Cerfa N° 51706#02 and N° 14906*02; in particular ARTICLES R. 214-87 to 214-137 from CODE RURAL ET DE LA PÊCHE MARITIME (French Regulation).
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