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Presser, K., Szymanek, J., Zoani, C., Castanheira, I.
Development of a Data Management Plan for METROFOOD-RI

METROFOOD-RI is a research infrastructure for promoting metrology in food and nutrition andis composed of a physical part where data is generated, and an electronic part where data can be accessed and used. This data includes information on available reference materials, existing reference and official methods, threshold values, proficiency testing as well as analytical data related to food composition, quality, safety, traceability and authenticity. In this work, the development of adata management plan (DMP)is presented to guarantee compliance and sustainability and to make data findable, accessible, interoperable and re- usable (FAIR). The DMP describesthe above-mentioned data entities in detail including source information, their format and define to whom it might be useful. It also defines that data can be stored on data owners’ side or in a central database.With respect to national and European data providers and their constraints, the DMP guarantees intellectual property rightsto data owners. Depending on the access policy of the data owner, certain data can be re-used, only be viewed or not be used at all by a certain user groups. Furthermore, the DMP contains a standard definition for the data format in which data should be exchanged and well-defined application programming interfaces (APIs) used for machine-to-machine communication.The data model behind the format and the APIs provide a harmonisation and standardisation of the data and allows data usage across Europe and beyond.The DMP also provides a data quality schemeto classify and assess data entering the METROFOOD-RI.

Borgese, L., Dalipi, R., Zoani, C., Zappa, G., Depero, L. E.
Multi-elemental Analysis of Oysters by Means of Total Reflection X-ray Fluorescence

Bivalves like oysters, clams and musselsare known to accumulate high amounts of metals. For this reason, they have been largely used as bio indicators. However, due to the toxic effects of some elements (As, Cd, Cr and Pb) at even the lowest concentrations, they are also analyzed for food safety purposes.
Generally, atomic spectrometry techniques, as inductively coupled plasma emission spectrometry (ICP-AES) and flame atomic absorption spectrometry (FAAS), are employed for element determination in biological samples. Anyhow, the use of these techniques requires sample preparation procedures for destruction of the organic matrix by chemical treatments. Sample digestion is a critical step in most of the analytical methods and furthermore it is time-consuming and losses of analytes by volatilization may happen.
Another technique that can be successfully used for elemental determination is total reflection X-ray fluorescence (TXRF) spectrometry. In this contribution, different reference freeze dried oyster samples provided by Italian Agency for New Technologies, Energy and Sustainable Economic Development (ENEA) were analyzed. Multi-elemental determination was performed by means of a low-power benchtop TXRF system. The analytical methodology developed consisted in simply suspending the powdered samples in a disperser agent. This procedure is faster, easier and does not involve the use of dangerous reagents.
The results that we have achieved with the present methodology were compared with the analysis of samples after microwave digestion. To evaluate the accuracy of the results, ICP-MS analysis of digested samples was also performed.

Alexandre, J., Tangni, E., Zoani, C., Donard, O., Van Loco, J.
METROFOOD-RI: inventory of the facilities and organization of the Physical Infrastructure

METROFOOD-RI is a Research Infrastructure (RI) for Promoting Metrology in Food and Nutrition composed by a Physical (P-RI) and an electronic (e-RI) infrastructure which are strictly interconnected. PRO-METROFOOD Project (H2020 INFRADEV-02-2016, GA n.739568) represents the “Early Phase” of the RI and has among its objectives the definition of the operational capacities of the P- RI, with the design of its scientific services. The facilities have been inventoried and classified in a database, which provides an organized overview of the capacities of the distributed P-RI.

Jitaru, P., Chekri, R., Lavison-Bompard, G., Fisicaro, P., Seby, F., Vacchina, V., Guérin, T., Donard, O.
PRO-METROFOOD Project: Involment of the French Node in setting up a novel European Research Infrastructure in Food and Nutrition

A French node constituted of four representative research institutes in Food chemistry are currently taking part to a consortium of 35 partners from 17 countries within the framework of a H2020-INFRADEV project (PRO-Metrofood). The main purpose of the PRO-Metrofood project is the preparation of the road map for the creation of a European Infrastructure for promoting Metrology in Food and Nutrition within the framework of the European Strategy Forum on Research Infrastructures (ESFRI).
All the French partners have excellent experience in high quality chemical measurement in foodstuff being involved in various joint research projects including PhD theses. They are involved in the PRO-Metrofood project as major actors of the same work-package: Technical Feasibility Study (WP4). A brief description of the French institutes taking part to the PRO-Metrofood project is provided below.
(i) The French Agency for Food, Environmental and Occupational Health & Safety (ANSES) undertakes monitoring, expert appraisal, research and reference missions in a broad field of competence that encompasses human health, animal health and welfare, and plant health. (ii) The French National metrology Institute (Laboratoire national de métrologie et d'essais, LNE) is a research infrastructure bringing the expertise in support of the reliability and comparability of analytical data. This will imply the provision of reference values for the certification of reference materials and for proficiency testing schemes as well as quality assurance tools mainly applied to the fields of inorganic and organic contaminations and nanoparticles characterisation. (iii) Université de Pau et des Pays de l'Adour (UPPA) contributes to the PRO-Metrofood project by means of the Center of Mass Spectrometry for Reactivity and Speciation Sciences (MARSS) which is an analytical platform integrated in the Institute of Analytical Sciences for Environmental and Material Sciences (IPREM). (iv) Ultra Traces Analyses Aquitaine (UT2A) is a spin-off of the IPREM having a large panel of expertise in trace metals measurements as well as characterization of nanoparticles in foodstuff.
This work presents the involvement of the French node in the WP4 of the PRO-Metrofood project whose main objectives are to list, structure and organize the facilities, expertise and know-how of the P-RI with respect to analyses, as well as to food production and qualification. This organization will also concern the full quality control of the chain starting from the production of reference materials to the advanced analytical facilities. In practical terms, the French node will carry out characterization of chemical contamination of three food matrices (rice grains, rice powder and oyster tissue) in terms of trace metals (including speciation) and organic contaminants (pesticides). The study will contribute to the production of several reference materials which will be used for methods validation and inter-laboratory comparisons by the partners of the PRO-Metrofood consortium.

Nevigato, T., Masci, M., Turrini, A., Caproni, R.
Comprehensive Analysis of Fatty Acids in Oysters by GC-FID/GC-MS

To the analysis of fatty acids in marine biota are generally related some uncertainties. One problem is that most profile analyses reported in literature disagree about the number and type of fatty acids monitored as well as about the percentage to assign to their sum over total fatty acids. Another issue is the discriminant effect in the split/splitless injector of gas chromatographs which can lead to relevant errors in quantifying DHA (22:6 ω3). In a previous work we solved these troubles for 12 fish species. In the present one the case of bivalve mollusks (oysters, mussels) is dealt with. Oysters are part of the analytical activity for producing a new Reference Material within the H2020 Project “PRO-METROFOOD”.

Masci, M., Nevigato, T., Turrini, A., Caproni, R.
Food Contamination by Organochlorines: Analysis of Oyster Tissue

Organochlorines (OCs) such as OC pesticides and polychlorobiphenyls are widespread toxic contaminants in the food chain, especially in aquatic biota. Despite they were banned by many years in western countries they still represent a topic of concern as addressed in the Stockholm Convention on Persistent Organic Pollutants (POPs) currently in force. The analyses of POPs at trace level in biological matrices may represent a challenge: if not properly conducted they may suffer of great uncertainties. In the present work the international guidelines about Good Laboratory Practice are strictly followed to analyse oysters and mussels. Other analytical innovations, recently developed in our laboratory, were applied in order to further improve accuracy. The oyster tissue is part of the analytical activity for producing a new Reference Material within the H2020 Project “PRO-METROFOOD”.

Winkelmann, O., Kuechler, T., Tsimidou, M., Nenadis, N., Mastralexi, A., Bendini, A., Gonzalez, D. L. G., Gallina Toschi, T.
Tailored sample preparation for olive oil Analysis by 1 H-NMR: Applications in sensory evaluation, origin classification and polyphenol determination

The 1H-NMR analysis of olive oil after dilution in CDCl3 has been exhaustively described in many scientific studies already. Due to the inherently low sensitivity of NMR, this approach provides little information about minor components present in the sample like polyphenols and volatiles.
An alternative sample preparation technique was developed and tested for its potential in addressing three important analytical issues. By employing a simple extraction with acetonitrile, a drastic enrichment of polyphenols and other polar compounds can be achieved. 1H-NMR analysis of these extracts can be used to classify olive oils according to geographical origin with striking success. In addition, markers attributable to the different sensory defects can be detected by the newly developed method, as demonstrated by the analysis of a large sample set of oils of different quality grades (extra virgin, virgin, lampante) which were assessed in parallel by sensory analysis. Affording extracts enriched in polyphenols, the method can also be used to determine the amount of polyphenols present in the oil. Employing the determination of phenolic content by the Folin Ciocalteu method, PLS-regression was used to predict the phenolic content from the NMR spectra. A high correlation between NMR data and the results from Folin Ciocalteu method was observed.
This work was developed in the context of the project OLEUM “Advanced solutions for assuring authenticity and quality of olive oil at global scale“ funded by the European Commission within the Horizon 2020 Programme (2014–2020, grant agreement no. 635690).

García González, D. L., Tena, N., Valli, E., Winkelmann, O., Brereton, P., Lacoste, F., Maquet, A., Vichi, S., Conte, L., Bendini, A., Gallina Toschi, T.
The development of Reference Materials in virgin olive oil sensory assessment: The contribution of Flavour Chemistry

The panel test is the standard method described by the current international regulations (e.g. norms from the International Olive Council) to assess sensory quality of virgin olive oil. At present, an intense discussion is centred in the need for the standardization of a method to be used in the assessment of the organoleptic characteristics in addition to the established panel test, as well as in the required improvement of the latter. In both cases, the existing knowledge on volatile compounds has to be applied and the development of reference materials are needed for increasing the metrological quality of the methods. Since there is existing knowledge about the volatile compounds responsible for some of the most common sensory defects (e.g. winey-vinegary), these compounds can be evaluated in their ability for producing reference materials associated to each sensory defect. For this purpose, these compounds have to be present in virgin olive oil characterized with sensory defects and a direct relationship between their occurrence and their sensory impact has to be demonstrated. The sensory properties of volatile compounds (attributes and odour thresholds) will be relevant to select volatile markers of the sensory defects that can form part of the formulation of reference materials. This work is being addressed in the project OLEUM “Advanced solutions for assuring authenticity and quality of olive oil at global scale” funded by the European Commission within the Horizon 2020 Programme (2014–2020, grant agreement no. 635690).

Valli, E., Palagano, R., Berardinelli, A., Ragni, L., Moreda, W., Pérez, Camino M., Bendini, A., Gallina Toschi, T.
Time Domain Reflectometry as a promising analytical approach for the determination of fatty acid ethyl esters in extra virgin olive oils

Fatty acid ethyl esters (FAEEs) are important quality and genuineness parameters for extra virgin olive oils (EVOOs), since they are considered i) direct markers strongly related to the quality of the olives and ii) possible indirect markers of an illegal soft-deodorization treatment. The EU Reg. 2095/2016 fixes the actual limit for FAEEs at 35 mg/kg for the commercial category of EVOO; the official EU analytical method for their determination in olive oil is particularly time consuming, so robust, rapid, and environmental friendly approaches for a preliminary screening of samples could be highly desirable. In this context, a set of extra virgin, virgin and lampante olive oils was considered. Firstly the content in FAEEs has been determined by following the EU official method. In parallel, all the samples were also analyzed by Time Domain Reflectometry (TDR) and waveforms were elaborated by Partial Least Squares multivariate regression (PLS). Test set validations procedures were considered. The aim was to build up-loadable models for the prediction of FAEEs, employing the data coming from conventional techniques for the calibration. Discriminant multivariate data analysis was also explored to classify samples. This approach is devoted to develop a prototype for validating the screening procedure. This work was developed in the context of the project OLEUM “Advanced solutions for assuring authenticity and quality of olive oil at global scale“ funded by the European Commission within the Horizon 2020 Programme (2014–2020, grant agreement no. 635690).

Gallina Toschi, T., Conte, L., García González, D., Maquet, A., Brereton, P., Fernández Celemín, L.
The EU H2020 OLEUM Project: state of play and advancements


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