MedOOmics Mediterranean Extra Virgin Olive Oil Omics: profiling and fingerprinting

Transcription

1 RIMNet2 Mid-Term Project Evaluation Meeting 12 October 2017, Montpellier, France MedOOmics Mediterranean Extra Virgin Olive Oil Omics: profiling and fingerprinting Coordinator Maria João CBRIT Universidade de Évora, Portugal 1

2 CONSORTIUM Project start date: 01/09/ Project end date: 31/08/2019 Universidade de Évora (Portugal) (Coordinator): stable isotopes, mineral elements and NMR Spectroscopy Universidade Nova de Lisboa - Portugal: comprehensive two-dimensional gas chromatography (if needed) dana Science and Technology University- Turkey: minor compounds of olive oil Cukurova University - Turkey: minor compounds of olive oil ix-marseille Université, France: chemometric and statistical techniques, Raman and Infrared Spectroscopy Centre Technique de l Olivier, France: sampling French olive oils Institut Supérieur de Biotechnologie de Sfax, Universite de Sfax, Tunisie: major compounds of olive oils

3 PROJECT OBJECTIVES Objective 1 full characterization of varietal EVOOs from Portugal, France, Turkey and Tunisia, targeting some less studied and typical varieties of each country. Objective 2 Establish tools that enable to ascertain the geographical origin of EVOOs, that can be further used for Geographical Indication of Origin (IGP) and Protected Designation of Origin (PDO) certification

4 PROJECT OBJECTIVES Objective 3 Establish chemical markers to be used for EVOOs authenticity Objective 4 Transfer of some methodologies developed within this proposal to industries

5 SCIENTIFIC PPROCH Profiling ICP/MS SIRMS HPLC-DD;HPLC-FLD; HPLC/MS GC/MS; GC x GC Fingerprinting NMR MIR NIR Raman

6 6 cultivars 2 or 3 areas STUDY RE / SITES 6 cultivars 1 or 2 areas 5 cultivars 1 or 2 areas 7 cultivars 1 or 2 areas

7 CTIVITIES / WORK PCKGES WP1 olive oil samples WP2 sensorial analysis WP3 - chemical characterization WP4 mineral elements determination WP7 Data treatment WP5 specroscopic profiles WP8 Results dissemination WP6 stable isotopic ratio analysis WP9 Management

8 Olive Oil samples (W1) France glandau, Picholine, Salonenque, Cailletier, Tanche, Olivière Portugal Cobrançosa, Galega Vulgar, Cordovil de Serpa, Blanqueta, Verdeal e Madural RESULTS SO FR Tunisia Oueslati, Zarrazi, Jemri, Zalmati, Neb Jmal, Chemlali, Chétoui Turkey Halhali, Hasebi, Kilis, Nizip, Sariulak

9 RESULTS SO FR OLIVE OIL TSTING PNELS (W2 -Tunisia) panel is established (following IOC standards) for organoleptic assessment of virgin olive oil form Tunisia, Portugal, France Turkey Chemlali Oueslati Vinou s Musty 2,5 2 1,5 1 0,5 Fruity 3 0 Bitter Punge nt Vinous Musty Fruity 3 2,5 2 1,5 1 0,5 0 Bitter Pungent Rancid Other s Rancid Others

10 RESULTS SO FR OLIVE OIL TSTING PNELS (W2 -Tunisia) Cobrançosa Fruity 6 Galega Vulgar Fruity 4 Musty 4 Bitter Musty 3 2 Bitter 2 1 Vinous 0 Pungent Vinou s 0 Punge nt Rancid Others Ranci d Other s Salonenque Picholine Fruity 4 Fruity 5 Musty Bitter Musty Bitter Vinou s 0 Punge nt Vinous 0 Pungent Rancid Other s Rancid Others

11 RESULTS SO FR Chemical characterization (W3-Tunisia) Liquid and Gaz Chromatography methodology for analysis of Triglycerides and fatty acid composition were established Fatty cids (%) France Tunisia Portugal Picholine Salonenque C14 : Chemlali Oueslati Cobrançosa Galega Vulgar C16 : C16 :1w C17 : C17 :1w C18 : C18 :1w C18 :2w C18 :3w C20 : C20 :1w GS GIS C18:1/C18:

12 RESULTS SO FR Chemical characterization (W3-Turkey) LC-DD-ESI-MS/MS methodology for analysis of phenolic compounds is established identification of 14 phenolic compounds:3 phenolic alcohols, 4 phenolic acids, 1 phenolic aldehyde, 3 secoiridoids, and 3 flavones 75 and 938 mg/kg 72 and 228 mg/kg 60 and 176 mg/kg France Portugal Turkey

13 RESULTS SO FR Mineral elements (W4) Optimization of sample preparation of olive oils: Wet digestion in hot plate results in uncomplete digested samples. Micro-wave digestion on going experiments nalytical methodology: Ready to go Calibration curves are done

14 P C - 2 ( 1 5 % ) Raman bsorbance Spectroscopic profiles (W5) 0,2 0,1 0-0,1 RESULTS SO FR Raman acquisition conditions optimised MIR and NIR data bases obtained PC on MIR Spectra of Portuguese samples Scores M M M M M M M M M M -0,2-0,4-0,3-0,2-0,1 0 0,1 0,2 0,3 PC-1 (66%) BL CB CR G M VE : amostras do lentejo; M : amostras de tras os Montes Pretreatment : SNV M Samples French, Cultivars prediction (Cal = 62, Val = 31) Portuguese, Cultivars prediction (Cal = 29, Val = 15) French + Portuguese, Cultivars prediction (Cal = 90, Val = 47) Portuguese, Regions prediction (Cal = 16, Val = 9) PLS1-D predictions on MIR Spectra % correct % uncertain [ ] Pre-treatment 87.1% 9.7% none 96.2% 2.2% SG 1 st derivative (7 points, order 2) 74.4% 15.6% none 85.6% 8.9% SG 1 st derivative (7 points, order 2) 91.5% 6.6% none 96.3% 2.7% SG 1 st derivative (7 points, order 2) 100.0% 0.0% none Irradiation Time 5x20s 5x10s Wavenumber (cm -1 ) 5x1s Parameters 3 to 10 factors RMSEP = 0.20 to to 10 factors, RMSEP = 0.16 à to 7 factors, RMSEP = 0.09 to to 6 factors, RMSEP = 0.14 to to 10 factors RMSEP = 0.10 to to 10 factors RMSEP = 0.10 to factors, RMSEP = 0.28

15 RESULTS SO FR Spectroscopic profiles (W5) NMR acquisition conditions optimised NMR data base being built frança Trás-os- Montes frança Tunisia lentejo Portugal

16 RESULTS SO FR Stable isotopes (W6) Olive oil bulk analysis is being developed for oxygen isotopes Carbon isotopes almost complete for all samples. Data analysis is being processed.

17 DISSEMINTION CTIVITIES Project webpage - available soon, under construction Conferences and worshops: Project presentation in Science Day at Évora University - Portugal Discrimination variétale des huiles d olive vierges extra - France uthentication of Tunisian virgin olive oils using volatile compounds and chemometric analysis - Tunisia Evaluation of phenolic composition and antioxidant activity changes in olive flowers during development using HPLC/DD and LC- MS/MS. - Tunisia

18 TRINING & MOBILITY Mobility Members of Tunisia Team have been in Portugal PhD student Ons Rekik, GC/MS techniques Post-Doc Boutheina Gargouri, GC/MS techniques Training Master, PhD and Post-Doc students: Nuno Martins (post-doc), rona Pires (PhD student) Boutheina Gargouri (Post-Doc) strid MLECHUX (PhD student)

19 NEXT STEPS / PERSPECTIVES Olive oil sampling from 2017 Obtaining results from all tasks, data treatment, publication

20 PROJECT FUNDERS

21 Thank you for your attention!