WHAT HAS OLEUM DONE UP TILL NOW?
To enable European and international regulators and policy makers with insights, updates from the scientific experts and needs from the stakeholders that can feed the path of regulatory standards, norms and their harmonization:
- OLEUM partners published a position paper on normative failures and inappropriateness and on analytical methods drawbacks into a scientific journal as gold open access.
- A report on the common and emerging fraud cases has been finalized and a paper will be submitted to a scientific journal, as open access contribution.
- A protocol for the in-house validation of the analytical methods has been prepared; the selection of the four analytical methods and two sensory reference materials to be full validated was done; inter-laboratory experiments on these selected analytical methods and RMs are in course.
To enhance methodology for the organoleptic assessment by improving reproducibility and developing a conjoint instrumental and sensory quantitative enhanced procedure (Quantitative Panel Test), including the adoption of at least two sensory reference materials:
- A new “OLEUM decision tree” scheme was developed and published (Barbieri et al., 2020) with the aim to classify and characterize samples in order to use them for possible correlations with physical–chemical data and to monitor and improve the performance of panels.
- Samples were analyzed simultaneously by different instrumental techniques and the most relevant volatile compounds have been selected according to their sensory impact. Two shared protocols for the determination of volatile compounds (by SPME-GC-MS and SPME-GC-FID) and three analytical approaches (NMR, Flash-GC-e-nose and untargeted SPME-GC-MS) were tested as possible screening methods to support the IOC Panel test; the untargeted SPME-GC-MS method was proposed for full validation and an article focused on this approach has been published into a scientific journal (Quintanilla-Casas, 2020).
- Two new artificial sensory reference materials (for the winey-vinegary and rancid defects) have been formulated ad hoc to resemble the defects and assessed by the OLEUM sensory panels for the detection threshold evaluation; their full validation it is in course with the contribution of panels not involved as partners in the OLEUM project.
To investigate on the analytical methods for verifying the olive oil quality:
- A series of extra virgin olive oil mixtures under different conditions of storage are being analyzed with different analytical tools (NMR, FT-IR, fluorescence spectroscopy, HPLC-MS/DAD-FLD, HS-SPME-GC/MS/FID) to evaluate the freshness/quality deterioration.
- A selection of the analytical methods (e.g. UHPLC/HPLC-DAD/MS, LC-qTOF/MS) for the phenolic compounds determination (health claim) were tested with a set of selected samples covering a wide range of phenol concentrations; an in-house validated method for the determination of total hydroxytyrosol and tyrosol in virgin olive oils fits for the purpose of the health claim was published (Tsimidou et al., 2019). The pros of this recently published in house validated method are also discussed in another research paper (Tsimidou et al., 2019b).
- A research paper in which it is presented a portable battery-operated electronic system for a rapid measure of the olive oil free acidity was published (Grossi et al., 2019).
To revise existing methods and to identify novel analytical markers with the aim of developing and validating innovative analytical solutions for ensuring the olive oil authenticity (illegal blends between extra virgin olive oil and soft deodorized olive oil, and between olive oil and other vegetable oils):
- The involved OLEUM partners analyzed samples of illegal (soft-deodorized OOs and vegetable oils) and legal (vegetable oils) blends with olive oil and extra virgin olive oils and a paper in which it is applied a decisional trees on how to verify the olive oil percentage in declared blends has been published (Gómez-Coca et al., 2020). A method proposing the revision of the preparative step of the official method for the FAEEs separation was proposed and in-house validated, as well as a revised method for determining sterols to detect illegal blends of OOs with other vegetable oils.
- Extra virgin and virgin olive oils were analyzed for assessing the geographical origin (Single State, EU, non-EU countries). Several chromatographic and spectroscopic analysis were discussed in the deliverable D4.9, as well as many useful analytical markers to establish the conformity of label-declared geographical origin.
- An article has been published with the aims to evaluate sesquiterpene hydrocarbons (SHs) as markers of EVOO geographical origin and to compare the discrimination efficiency of targeted profiling and fingerprinting approaches (Quintanilla-Casas et al., 2020).
To promote open-access knowledge generation and dissemination by making globally available all the information coming from OLEUM research:
- OLEUM Databank was launched and an implementation will be made in terms of definition of IPR and uploading of contents. A sustainability plan will be also defined for the subsequent maintenance of the OLEUM Databank after the end of the project.
To undertake technology transfer of new methods and procedures to a wide analytical community and to assess its proficiency by specific fit-for-purpose actions (e.g. analytical discussions, needs of ring tests):
- Full validation and technology transfer processes are in course for four methods: 1) method to detect blends of EVOOs with soft-deodorized OOs with a revision of the preparative step of the FAEEs separation; 2) revised method to determine free and esterified sterols to detect illegal blends of OOs with other vegetable oils; 3) method for the determination of the phenolic compounds (health claim); 4) Quantitative Panel Test.
- Two Training Workshops were successfully held (first in Seville and the second in Bologna) with the aim of receiving technical feedbacks before submitting the methods to the full validation process (trial propers).
To engage the widest range of stakeholders (opinion leaders/regulators, food and drink industries including SMEs, the media, the scientific community, consumers) in the dissemination, exploitation and knowledge exchange:
- The OLEUM Network has followed two complementary approaches: a LinkedIn group (OLEUM question of the months) for general aspects relating to the quality and authenticity of olive oil (over 100 members up to now) and a secure network (Basecamp) for those involved in the laboratory analysis of olive oil (more than 60 members up to now).
- An infographic for public dissemination on the production of olive oil and one on how to recognize a good quality extra virgin olive oil were realized, as well as a short video presenting the project was produced.
All activity, results and achievements of OLEUM during the previous years, can be found here.
REFERENCES
Barbieri S., Brkić Bubola K., Bendini A., Bučar-Miklavčič M., Lacoste F., Tibet U., Winkelmann O., García-González D.L., Gallina Toschi T. 2020. Alignment and proficiency of virgin olive oil sensory panels: the OLEUM Approach. Foods, 9, 355, DOI: 10.3390/foods9030355
Conte L., Bendini A., Valli E., Lucci P., Moret S., Maquet A., Lacoste F., Brereton P., García-Gonzáles D. L., Moreda W., Gallina Toschi T. 2019. Olive oil quality and authenticity: A review of current EU legislation, standards, relevant methods of analyses, their drawbacks and recommendations for the future. Trends in Food Science & Technology, DOI: 10.1016/j.tifs.2019.02.025. En proceso de impresión.
Gallina Toschi T., Valli E., Conte L., García-Gonzáles D. L., Maquet A., Brereton P., Mcgrath N., Celemín L. F., Bendini A. 2017. EU project OLEUM: Better solutions to protect olive oil quality and authenticity. Agro Food Industry Hi-Tech 28 (5), pp. 2-3, https://zenodo.org/record/1184863#.WsccF5e-lPY
Gómez-Coca R.B., Pérez-Camino M.C., Martínez-Rivas J.M., Bendini A., Gallina Toschi T., Moreda W. 2020. Olive oil mixtures. Part one: Decisional trees or how to verify the olive oil percentage in declared blends. Food Chemistry, 315, 126235, DOI: 10.1016/j.foodchem.2020.126235
Grossi M., Palagano R., Bendini A., Riccò B., Servili M., García-González D. L., Gallina Toschi T. 2019. Design and in-house validation of a portable system for the determination of free acidity in virgin olive oil. Food Control 104, pp. 208–216, DOI: 10.1016/j.foodcont.2019.04.019.
Quintanilla-Casas B., Bertin S., Leik K., Bustamante J., Guardiola F., Valli E., Bendini A., Gallina Toschi T., Tres A., Vichi S. 2020. Profiling versus fingerprinting analysis of sesquiterpene hydrocarbons for the geographical authentication of extra virgin olive oils. Food Chemistry, 307,125556, DOI: 10.1016/j.foodchem.2019.125556
Quintanilla-Casas B., Bustamante J., Guardiola F., García-González D.L., Barbieri S., Bendini A., Gallina Toschi T., Vichi S., Tres A. 2020. Virgin olive oil volatile fingerprint and chemometrics: towards an instrumental screening tool to grade the sensory quality. LWT – Food Science and Technology, 121, 108936, DOI: 10.1016/j.lwt.2019.108936
Tsimidou M. Z., Nenadis N., Servili M., García-Gonzáles D. L., Gallina Toschi T. 2018. Why tyrosol derivatives have to be quantified in the calculation of “olive oil polyphenols” content to support the health claim provisioned in the EC Reg. 432/2012. European Journal of Lipid Science and Technology, 120(6),1800098, DOI: 10.1002/ejlt.201800098.
Tsimidou M. Z., Sotiroglou M., Mastralexi A., Nenadis N., García-González D. L., Gallina Toschi T. 2019. In House Validated UHPLC Protocol for the Determination of the Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil Fit for the Purpose of the Health Claim Introduced by the EC Regulation 432/2012 for “Olive Oil Polyphenols”. Molecules 24, 1044, DOI:10.3390/molecules24061044.
Tsimidou M. Z., Nenadis N., Mastralexi A., Servili M., Butinar B., Vichi S., Winkelmann O., García-Gonzáles D. L., Gallina Toschi T. 2019b. 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). Molecules 24, 2429, DOI:10.3390/molecules24132429.
Nenadis N., Mastralexi A., Tsimidou M.Z., Vichi S., Quintanilla-Casas B., Donarski J., Bailey-Horne V., Butinar B., Miklavčič M., García González D.-L., Gallina Toschi T. 2018. Toward a Harmonized and Standardized Protocol for the Determination of Total Hydroxytyrosol and Tyrosol Content in Virgin Olive Oil (VOO). Extraction Solvent. European Journal of Lipid Science and Technology, DOI: 10.1002/ejlt.201800099