Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) Procedure

Τoward a harmonized and standardized procedure for the determination of total hydroxytyrosol and tyrosol content in virgin olive oil (VOO), the pros of a recently published in house validated ultra high performance liquid chromatography (UHPLC) protocol are discussed comparatively with thos...

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Main Authors: Maria Z. Tsimidou, Nikolaos Nenadis, Aspasia Mastralexi, Maurizio Servili, Bojan Butinar, Stefania Vichi, Ole Winkelmann, Diego Luis García-González, Tullia Gallina Toschi
Format: Article
Language:English
Published: MDPI AG 2019-07-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/24/13/2429
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author Maria Z. Tsimidou
Nikolaos Nenadis
Aspasia Mastralexi
Maurizio Servili
Bojan Butinar
Stefania Vichi
Ole Winkelmann
Diego Luis García-González
Tullia Gallina Toschi
author_facet Maria Z. Tsimidou
Nikolaos Nenadis
Aspasia Mastralexi
Maurizio Servili
Bojan Butinar
Stefania Vichi
Ole Winkelmann
Diego Luis García-González
Tullia Gallina Toschi
author_sort Maria Z. Tsimidou
collection DOAJ
description &#932;oward a harmonized and standardized procedure for the determination of total hydroxytyrosol and tyrosol content in virgin olive oil (VOO), the pros of a recently published in house validated ultra high performance liquid chromatography (UHPLC) protocol are discussed comparatively with those of other procedures that determine directly or indirectly the compounds hosted under the health claim on &#8220;olive oil polyphenols&#8221; (EC regulation 432/2012). Authentic VOOs were analyzed with five different liquid chromatographic separation protocols and <sup>1</sup>H-NMR one in five different laboratories with expertise in VOO phenol analysis within three months. Data comparison indicated differences in absolute values. Method comparison using appropriate tools (Passing-Bablok regression and Bland Altman analyses) for all protocols vs. the UHPLC one indicated slight or statistically significant differences. The results were also discussed in terms of cost effectiveness, detection means, standard requirements and ways to calculate the total hydroxytyrosol and tyrosol content. Findings point out that the in-house validated fit for the purpose UHPLC protocol presents certain pros that should be exploited by the interested parties. These are the simplicity of sample preparation, fast elution time that increase the number of samples analyzed per day and integration of well-resolved peaks with the aid of only two commercially available external standards. Importance of correction factors in the calculations is stressed.
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spelling doaj.art-f0042873eac842a2ba578042b1cc06822022-12-22T00:33:27ZengMDPI AGMolecules1420-30492019-07-012413242910.3390/molecules24132429molecules24132429Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) ProcedureMaria Z. Tsimidou0Nikolaos Nenadis1Aspasia Mastralexi2Maurizio Servili3Bojan Butinar4Stefania Vichi5Ole Winkelmann6Diego Luis García-González7Tullia Gallina Toschi8Laboratory of Food Chemistry and Technology, School of Chemistry, Aristotle University of Thessaloniki (AUTH), 541 24 Thessaloniki, GreeceLaboratory of Food Chemistry and Technology, School of Chemistry, Aristotle University of Thessaloniki (AUTH), 541 24 Thessaloniki, GreeceLaboratory of Food Chemistry and Technology, School of Chemistry, Aristotle University of Thessaloniki (AUTH), 541 24 Thessaloniki, GreeceDepartment of Agricultural, Food and Environmental Sciences, University of Perugia, (UNIPG), Via San Costanzo s.n.c., 06126 Perugia, ItalyLaboratory of the Institute for Oliveculture, Science and Research Centre Koper (ZRS), Zelena ulica 8k, SI-6310 Izola, SloveniaDepartment de Nutrició, Ciències de l’Alimentació i Gastronomia, XaRTA, INSA-UB, Campus De l’Alimentació Torribera, Universitat de Barcelona (UB), Av. Prat de la Riba, 171, 08028 Santa Coloma de Gramenet, SpainEurofins Analytik GmbH, Neuländer Kamp 1, 21079 Hamburg, GermanyInstituto de la Grasa (CSIC), Ctra. De Utrera, km. 1, Campus Universitario Pablo de Olavide—Building 46, 41013 Seville, SpainDepartment of Agricultural and Food Sciences, Alma Mater Studiorum, University of Bologna (UNIBO), Piazza Goidanich, 60, I-47521 Cesena (FC), Bologna, Italy&#932;oward a harmonized and standardized procedure for the determination of total hydroxytyrosol and tyrosol content in virgin olive oil (VOO), the pros of a recently published in house validated ultra high performance liquid chromatography (UHPLC) protocol are discussed comparatively with those of other procedures that determine directly or indirectly the compounds hosted under the health claim on &#8220;olive oil polyphenols&#8221; (EC regulation 432/2012). Authentic VOOs were analyzed with five different liquid chromatographic separation protocols and <sup>1</sup>H-NMR one in five different laboratories with expertise in VOO phenol analysis within three months. Data comparison indicated differences in absolute values. Method comparison using appropriate tools (Passing-Bablok regression and Bland Altman analyses) for all protocols vs. the UHPLC one indicated slight or statistically significant differences. The results were also discussed in terms of cost effectiveness, detection means, standard requirements and ways to calculate the total hydroxytyrosol and tyrosol content. Findings point out that the in-house validated fit for the purpose UHPLC protocol presents certain pros that should be exploited by the interested parties. These are the simplicity of sample preparation, fast elution time that increase the number of samples analyzed per day and integration of well-resolved peaks with the aid of only two commercially available external standards. Importance of correction factors in the calculations is stressed.https://www.mdpi.com/1420-3049/24/13/2429virgin olive oilhydroxytyrosoltyrosolhealth claimEuropean Commission Regulation 432/2012standardizationUHPLC-DADHPLC-DADLC-HRMS<sup>1</sup>H-NMR spectroscopy
spellingShingle Maria Z. Tsimidou
Nikolaos Nenadis
Aspasia Mastralexi
Maurizio Servili
Bojan Butinar
Stefania Vichi
Ole Winkelmann
Diego Luis García-González
Tullia Gallina Toschi
Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) Procedure
Molecules
virgin olive oil
hydroxytyrosol
tyrosol
health claim
European Commission Regulation 432/2012
standardization
UHPLC-DAD
HPLC-DAD
LC-HRMS
<sup>1</sup>H-NMR spectroscopy
title Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) Procedure
title_full Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) Procedure
title_fullStr Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) Procedure
title_full_unstemmed Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) Procedure
title_short Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). The Pros of a Fit for the Purpose Ultra High Performance Liquid Chromatography (UHPLC) Procedure
title_sort toward a harmonized and standardized protocol for the determination of total hydroxytyrosol and tyrosol content in virgin olive oil voo the pros of a fit for the purpose ultra high performance liquid chromatography uhplc procedure
topic virgin olive oil
hydroxytyrosol
tyrosol
health claim
European Commission Regulation 432/2012
standardization
UHPLC-DAD
HPLC-DAD
LC-HRMS
<sup>1</sup>H-NMR spectroscopy
url https://www.mdpi.com/1420-3049/24/13/2429
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