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Th Èse D E D O Cto Implementation of a physio- chemical approach coupled with a data fingerprinting methodology for the characterization of the Lebanese extra-virgin olive oils Thèse de doctorat de l'université Paris-Saclay École doctorale n° 581, Agriculture, alimentation, biologie, environnement et santé (ABIES) Spécialité de doctorat : Chimie Analytique Unité de recherche : Université Paris-Saclay, AgroParisTech, INRAE, UMR PNCA, 75005, Paris, France. Référent : AgroParisTech Thèse présentée et soutenue à Paris-Saclay, le 28/01/2021, par Omar DIB Composition du Jury Olivier DONARD Président Directeur de Recherche, CNRS (Université de Pau) Nathalie DUPUY Rapporteur & Examinatrice Professeur, Université Aix-Marseille Imad TOUFEILI Rapporteur & Examinateur Professor, American University of Beirut 4 Jérôme VIAL Examinateur Maitre de Conférences, ESPCI – PSL Université ASB00 Christophe CORDELLA Directeur de thèse Ingénieur de Recherche, INRAE (Centre Jouy-en-Josas) UP 1 ALi BASSAL Co-Directeur & Examinateur Professor, Lebanese University : 202 Luc EVELEIGH Co-Encadrant & Examinateur Maître de Conférences, AgroParisTech Rita YAACOUB NNT Co-Encadrante & Examinatrice Thèse de doctorat Associate Professor, Lebanese University 2 Acknowledgments This work was carried out in Lebanon (Faculty of Agricultural Sciences, Lebanese University) and in France (Laboratoire de Chimie Analytique, AgroParisTech) under the supervision of Prof. Ali Bassal and Dr. Christophe Cordella. To whom I address my sincere thanks and gratitude for their scientific advice and encouragement. Thank you from the bottom of my heart for directing me throughout this thesis. Never to mention your support and, above all, your confidence in me. My respectful gratitude to CNRS-Lebanon and Lebanese University (UL) for their financial support throughout the whole Ph.D. program. I would like to thank the ABIES Doctoral School and its director Dr. Alexandre Perry and the EDST doctoral school, and its Dean, Dr. Omar Fawaz. Without them, my journey as a Ph.D. candidate wouldn’t be possible. My thanks go to the jury members Dr. Nathalie Dupuy, Dr. Imad Toufeili, Dr. Olivier Donard, and Dr. Jérôme Vial, for giving the time to criticize and improve my work and for accepting to be members of the defense committee. I won’t forget my thesis committee, which accompanied me throughout the work. My sincere thanks to Dr. Rita Yaacouub and Dr. Luc Eveleigh for granting their time and assistance in realizing this work. Thank you for always being there to help me and for answering my questions. I express my deep gratitude to Dr. Ali Toufeil, Dr. Audrey Solgadi and Dr. Milad Riyachi. Thank you for welcoming me to the SAMM and LARI Laboratories and for giving the time to pass on the knowledge of spectroscopy, chromatography and olive oil extraction. My thanks also go to Dr. Jad Rizkalah for providing me with his knowledge of statistical studies and MATLAB software. Thank you for offering your help, answer my questions, and for all the advice over the years. I would also like to thank all the laboratory members and assistants, particularly Mrs. Nathalie Locquet and Mr. Ghassan Menhem, for their technical assistance. A big thank you to the AgroParisTech team, Prof. Douglas Rutledge, Dr. Delphine Bouveresse, Roberto Garcia, Yann Padellec, Camille Cassin, and Dr.Hervé This. Thank you, Marguerite, Rita, Layth, Hisham, Sophia, Tala, Dina, Ola, Grégoire, Miguel, Béninia, Fransesc, Antoine, Alberto, Emma, Lilhou, Bastien, Marie-Charlotte, James, Asma and Daniela. I will never forget your support and the good times we had together. My affection goes to my family, Dad, Mom, and my brothers, who have supported me throughout these years. I hope you will always be in good health. Be sure I will always make you proud, in Lebanon, France, or any other country in the world. Because of you, I have found the strength to face all obstacles and make it this far. A special thanks to Dr. Hussein Dib, my Dad, my Mentor and soon my colleague. Without you and your continuous support, I could not have made it through this challenging experience. I love you all! 3 ُ ْ َ َ ُ َ ْ Allah is the Light of the heavens and the earth. The* * ﱠ&ُ ﻧ ُﻮر ﱠاﻟﺴ ِﻤﺎوات واﻷ ْر ِض َﻣﺜ ُﻞ ﻧ ِﻮر ِه ﻛ ِﻤﺸﻜﺎةٍ ﻓِﯿﮭﺎ example of His light is that of a niche, in which there ْ ُ َ ِﻣ ْﺼ ٌﺒﺎح اﻟ ِﻤ ْﺼ ُﺒﺎح ﻓِﻲ ُز َﺟﺎﺟ ٍﺔ ﱡاﻟﺰ َﺟﺎﺟﺔ َﻛﺄﻧﱠﮭﺎ َﻛ ْﻮ َﻛ ٌﺐ is a lamp; the lamp is in a glass – the glass looks like a brilliant star – it is lit by (the oil of) a blessed tree, دُ ِّر ﱞي ﯾُﻮﻗَﺪُ ِﻣ ْﻦ َﺷ َﺠ َﺮةٍ ُﻣ َﺒﺎر َﻛ ٍﺔ َز ْﯾﺘُﻮﻧَ ٍﺔ ﻻ َﺷ ْﺮﻗِﯿﱠ ٍﺔ ﻻو the olive, which is neither eastern, nor western. Its oil َﻏ ْﺮﺑِﯿﱠ ٍﺔ ﯾَﻜﺎدُ َز ْﯾﺘُﮭﺎ ﯾُ ِﻀﻲ ُء وﻟَ ْﻮ ﻟَ ْﻢ ﺗَ ْﻤ َﺴ ْﺴﮫُ ٌﻧﺎر ﻧُ ٌﻮر is about to emit light even though the fire has not touched it – (it is) light upon light. Allah guides to َﻋﻠﻰ ﻧُ ٍﻮر ﯾَ ْﮭ ِﺪي ﱠ&ُ ِﻟﻨُ ِﻮر ِه َﻣ ْﻦ ﯾَ ُﺸﺎء وﯾَ ْﻀ ِﺮ ُب ﱠ&ُ His light whomsoever He wills; Allah describes ْاﻷَ ْﻣ َﺜﺎل ِﻟﻠﻨﱠ ِﺎس ﱠو&ُ ﺑِ ُﻜ ِّﻞ َﺷ ْﻲ ٍء َﻋ ِﻠ ٌﯿﻢ examples for the people, and Allah knows everything well. * آﺮﻟانﻘﺮ ،ﻟاﻢﯾﻜ رﻮﺳ ة ا ﻟ ﻨ رﻮ ، آ ﯾ ﺔ 35 ،ﺤﻔﺻ ﺔ Quran al Karim, An-Nur, Verse 35, Page 354 354* (Translated by: Mufti Taqi Usmani) 4 Table of Contents List of Formation ................................................................................................................. 9 List of Publications ............................................................................................................ 10 List of Abbreviations ......................................................................................................... 12 List of Symbols .................................................................................................................. 14 List of Figures .................................................................................................................... 16 List of Tables ..................................................................................................................... 17 General Introduction ......................................................................................................... 18 Chapter 1: Literature Review ............................................................................................. 23 1. A general overview on olive oil .................................................................................... 23 1.1. Olive oil: an introduction .................................................................................................... 23 1.2. Geographic distribution of olive oil production and consumption ....................................... 24 1.3. The rise of regulation .......................................................................................................... 25 1.4. Chemical Composition ........................................................................................................ 27 1.4.1. Fatty acids .......................................................................................................................................... 27 1.4.2. Sterols ................................................................................................................................................ 28 1.4.3. Polyphenols ........................................................................................................................................ 28 1.4.4. Chlorophylls ....................................................................................................................................... 28 1.4.5 Aromatic compounds .......................................................................................................................... 29 2. Lebanese olive oil sector overview .............................................................................. 31 2.1. Main Geographical features ................................................................................................ 31 2.2. Olive oil production ............................................................................................................ 32 2.3 Imports and exports ............................................................................................................ 33 3. Fluctuation of EVOO/VOO components due to factors of different origins ................... 34 3.1. Agronomical variables ........................................................................................................ 34 3.1.2. Climate and elevation ........................................................................................................................ 35 3.1.3 Fruit maturity ...................................................................................................................................... 36 5 3.1.4 Other agronomical factors .................................................................................................................. 37 3.2. Technological variables ....................................................................................................... 38 3.2.1. Olive transport and storage ............................................................................................................... 38 3.2.2. Processing methods ........................................................................................................................... 38 3.2.3. Storage conditions ............................................................................................................................. 41 4. Rapid & non-destructive analysis techniques ..............................................................
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