Virgin olive oil authenticity assays in a single run using two-dimensional liquid chromatography-high resolution mass spectrometry

Sterols and triterpenic alcohol analyses are one of the officially established parameters for assessing the authenticity of virgin olive oil. Most of the applications described for sterol analysis, including the official method, only allow the determination of the total sterol content but not its di...

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Detalles Bibliográficos
Autores: Caño-Carrillo, Irene, Gilbert-López, Bienvenida, Ruiz-Samblás, Cristina, Molina-Díaz, Antonio, García-Reyes, Juan F.
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2024
País:España
Institución:Universidad de Jaén
Repositorio:RUJA. Repositorio Institucional de la Producción Científica de la Universidad de Jaén
OAI Identifier:oai:ruja.ujaen.es:10953/6315
Acceso en línea:https://doi.org/10.1021/acs.analchem.4c03678
https://hdl.handle.net/10953/6315
Access Level:acceso abierto
Palabra clave:Two-dimensional liquid chromatography, mass spectrometry, olive oil, authenticity
2301.03
2301.10
Descripción
Sumario:Sterols and triterpenic alcohol analyses are one of the officially established parameters for assessing the authenticity of virgin olive oil. Most of the applications described for sterol analysis, including the official method, only allow the determination of the total sterol content but not its distribution in free or esterified form. This work proposes a two-dimensional liquid chromatography/high-resolution mass spectrometry (2D-LC-HRMS) method for the simultaneous analysis of triterpenic alcohols, free sterols and steryl esters. A RPLC-RPLC coupling was performed through a multiple heart-cutting (MHC) interface equipped with an active solvent modulation valve (ASM). Additionally, a selection valve was coupled to the 2D-LC system, allowing the simultaneous data acquisition from both dimensions in a single analysis. A simplified sample treatment based on solid phase extraction was also proposed to avoid tedious steps such as saponification or derivatization before GC analysis. To evaluate the content of these compounds in different olive oil categories, the proposed 2D-LC-HRMS system was applied to a set of samples from different commercial olive oil categories (EVOO, VOO, OO, POO) and sunflower oil. The results revealed significant differences in the distribution of free and esterified sterols of the analyzed samples, highlighting the free/esterified sterol ratio as a powerful tool to unveil olive oil fraud practices and fat manipulation.