Peer inter-laboratory validation study of a harmonized SPME-GC-FID method for the analysis of selected volatile compounds in virgin olive oils

Autor: Beatriz Quintanilla-Casas, Enrico Casadei, Stefania Vichi, Alba Tres, Clemente Ortiz-Romero, Ramón Aparicio-Ruiz, Enrico Valli, Diego L. García-González, Alessandra Bendini, Tullia Gallina Toschi
Přispěvatelé: European Commission, Ministerio de Ciencia, Innovación y Universidades (España), Agencia Estatal de Investigación (España), Enrico Casadei, Enrico Valli, Ramón Aparicio-Ruiz, Clemente Ortiz-Romero, Diego L. García-González, Stefania Vichi, Beatriz Quintanilla-Casas, Alba Tres, Alessandra Bendini, Tullia Gallina Toschi, Universidad de Sevilla. Departamento de Química Analítica, Universidad de Sevilla. AGR104: Proyecto Sexia
Rok vydání: 2020
Předmět:
Zdroj: Dipòsit Digital de la UB
Universidad de Barcelona
Digital.CSIC. Repositorio Institucional del CSIC
instname
Food Control
Popis: In the context of supporting the panel test in the classification of virgin olive oils, the qualitative and quantitative analysis of a number of volatile compounds responsible for their aroma is of great importance. Herein, the data obtained from three laboratories that analyzed the same samples are presented with the view to develop an inter-laboratory validation study of a harmonized solid-phase micro-extraction coupled with gas-chromatography with flame ionized detector (SPME-GC-FID) method for determination of selected volatile compounds. In particular, quantification of the minimum number of key markers responsible for positive attributes (e.g. fruity) and sensory defects was investigated. Three quantification strategies were considered since they can have a notable impact on the effectiveness of the use of markers as well as on the robustness and simplicity of the method that is designed for control laboratories. A peer-validation study indicated repeatability with a mean relative standard deviation (RSD%) lower than 14% except for ethyl propanoate, 3-methyl-1-butanol, 1-octen-3-ol, and (E)-2-decenal. Linearity was satisfactory (R2 > 0.90) for all compounds when the calibration curves were corrected by the internal standard. Several critical issues were identified, such as high RSD% (>50%) in terms of reproducibility for ethyl propanoate, (E)-2-decenal, and possible improvements of the limits of detection (LODs) and quantitation (LOQs) of (E)-2-heptenal, (E,E)-2,4-hexadienal, and (E)-2-decenal. In particular, some compounds (ethyl propanoate, (E)-2-heptenal, 1-octen-3-ol, (E,E)-2,4-hexadienal, (E)-2-decenal and pentanoic acid) showed LOQs that were higher than the concentrations found in some samples. The discussion permitted improvement of the protocol towards the final version for an upcoming full validation process.
This work was supported by the Horizon 2020 European Research project OLEUM “Advanced solutions for assuring the authenticity and quality of olive oil at a global scale”, which has received funding from the European Commission within the Horizon 2020 Programme (2014–2020), grant agreement no. 635690. The information expressed in this article reflects the authors’ views; the European Commission is not liable for the information contained herein. B. Quintanilla-Casas and A. Tres thanks the Spanish Ministry of Science, Innovation and Universities for a predoctoral (FPU16/01744) and a Ramón y Cajal (RYC-2017-23601) postdoctoral fellowship, respectively.
Databáze: OpenAIRE
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