Ion mobility-mass spectrometry to extend analytical performance in the determination of ergot alkaloids in cereal samples

Laura Carbonell-Rozas; Maykel Hernández-Mesa; Laura Righetti; Fabrice Monteau; Francisco J Lara; Laura Gámiz-Gracia; Bruno Le Bizec; Chiara Dall'Asta; Ana M García-Campaña; Gaud Dervilly

doi:10.1016/j.chroma.2022.463502

Ion mobility-mass spectrometry to extend analytical performance in the determination of ergot alkaloids in cereal samples

J Chromatogr A. 2022 Oct 25:1682:463502. doi: 10.1016/j.chroma.2022.463502. Epub 2022 Sep 14.

Affiliations

¹ Oniris, INRAE, LABERCA, 44300 Nantes, France; Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Campus Fuentenueva s/n, 18071 Granada, Spain.
² Oniris, INRAE, LABERCA, 44300 Nantes, France; Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Campus Fuentenueva s/n, 18071 Granada, Spain. Electronic address: maykelhm@ugr.es.
³ Department of Food and Drug, University of Parma, Parco Area delle Scienze 17/A, 43124 Parma, Italy.
⁴ Oniris, INRAE, LABERCA, 44300 Nantes, France.
⁵ Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Campus Fuentenueva s/n, 18071 Granada, Spain.

PMID: 36174373
DOI: 10.1016/j.chroma.2022.463502

Abstract

This work evaluates the potential of ion mobility spectrometry (IMS) to improve the analytical performance of current liquid chromatography-mass spectrometry (LC-MS) workflows applied to the determination of ergot alkaloids (EAs) in cereal samples. Collision cross section (CCS) values for EA epimers are reported for the first time to contribute to their unambiguous identification. Additionally, CCS values have been inter-laboratory cross-validated and compared with CCS values predicted by machine-learning models. Slight differences were observed in terms of CCS values for ergotamine, ergosine and ergocristine and their corresponding epimers (from 3.3 to 4%), being sufficient to achieve a satisfactory peak-to-peak resolution for their unequivocal identification. A LC-travelling wave ion mobility (TWIM)-MS method has been developed for the analysis of EAs in barley and wheat samples. Signal-to-noise ratio (S/N) was improved between 2.5 and 4-fold compared to the analog LC-TOF-MS method. The quality of the extracted ion chromatograms was also improved by using IMS.

Keywords: Cereal samples; Collision cross section; Ergot alkaloids; Ion mobility-mass spectrometry; Travelling wave ion mobility spectrometry.

MeSH terms

Edible Grain / chemistry
Ergot Alkaloids* / analysis
Ergotamines / analysis
Ion Mobility Spectrometry / methods
Mass Spectrometry / methods

Substances

Ergot Alkaloids
Ergotamines