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Fractionnement De Coproduits De Pin Maritime (Pinus Pinaster)

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Fractionnement De Coproduits De Pin Maritime (Pinus Pinaster) THÈSE En vue de l'obtention du DOCTORAT DE L’UNIVERSITÉ DE TOULOUSE Délivré par L’Institut National Polytechnique de Toulouse (INP Toulouse) Discipline ou spécialité Sciences des agroressources – CO019 Présentée et soutenue par M. Clément CELHAY le lundi 18 mars 2013 Titre : Fractionnement de coproduits de pin maritime (Pinus pinaster) et de peuplier (Populus tremula) pour l'obtention d'extraits polyphénoliques à activité antioxydante : procédé d'extraction aqueuse en extracteur bi-vis et étude des conditions subcritiques Ecole: doctorale Sciences de la Matière (SDM) Unité de recherche : Laboratoire de Chimie Agro-industrielle (LCA) Directeurs de Thèse : M. Gérard VILAREM - Ingénieur de Recherche - LCA - ENSIACET - INP Toulouse M. Luc RIGAL - Ingénieur de Recherche - LCA - ENSIACET - INP Toulouse Jury : M. Nicolas FABRE - Professeur - Faculté de Pharmacie - Université de Toulouse - Président M. Gilles LABAT - Ingénieur de Recherche - FCBA - Bordeaux - Membre M. Gérard VILAREM - Ingénieur de Recherche - LCA - ENSIACET - INP Toulouse - Membre M. Luc RIGAL - Ingénieur de Recherche - LCA - ENSIACET - INP Toulouse - Membre M. Farid CHEMAT - Professeur - Université d'Avignon et des Pays du Vaucluse - Rapporteur M. Rimantas VENSKUTONIS - Professeur - University of Kaunas - Lituanie - Rapporteur Sommaire Sommaire Remerciements de thèse ........................................................................................................... 7 Introduction générale ............................................................................................................. 13 Chapitre I : Les coproduits de l’industrie papetière, des matières riches en polyphénols et en antioxydants ................................................................................................................... 19 I.1. L’arbre ............................................................................................................................ 21 I.1.1. Deux grandes classes d’arbres .................................................................................. 21 I.1.1.1. Les résineux ...................................................................................................... 21 I.1.1.2. Les feuillus ....................................................................................................... 21 I.1.2. Structure externe de l’arbre : morphologie générale ................................................ 22 I.1.2.1. Le houppier ...................................................................................................... 22 I.1.2.2. Le tronc ............................................................................................................ 24 I.1.2.3. Le système racinaire ......................................................................................... 24 I.1.3. Structure interne de l’arbre : une superposition de feuillets ..................................... 24 I.1.3.1. L’écorce ............................................................................................................ 25 I.1.3.2. Le liber ............................................................................................................. 26 I.1.3.3. Le cambium ...................................................................................................... 26 I.1.3.4. L’aubier et le bois de cœur ............................................................................... 26 I.1.3.4.1. L’aubier .................................................................................................... 26 I.1.3.4.2. Le bois de cœur ........................................................................................ 27 I.2. La filière bois en France et en Europe .......................................................................... 27 I.2.1. Les activités de la filière bois en France .................................................................. 28 I.2.2. Des coproduits générés en grandes quantités ........................................................... 29 I.2.3. Valorisation directe des coproduits du bois ............................................................. 31 I.2.4. Les principales essences de l’industrie papetière : le pin maritime et le peuplier européen ............................................................................................................................... 32 I.2.4.1. Localisation, caractéristiques botaniques et utilisation du pin maritime.......... 33 I.2.4.2. Localisation, caractéristiques botaniques et utilisation du peuplier européen . 34 I.2.4.3. Valorisation indirecte des coproduits du bois .................................................. 36 I.3. Les nœuds et les écorces d’arbres, sources de composés bioactifs ............................. 36 I.3.1. Les constituants de la matrice végétale .................................................................... 37 I.3.1.1. Les constituants des parois végétales : cellulose, hémicelluloses et lignines .. 37 I.3.1.2. Les protéines et l’azote ..................................................................................... 39 I.3.1.3. Les composés lipophiles et les résines ............................................................. 40 I.3.1.4. Les extractibles hydrophiles ............................................................................. 40 I.3.1.5. Polyphénols et antioxydants naturels, des composés phytochimiques d’intérêt .. .......................................................................................................................... 42 I.3.1.5.1. Les polyphénols ........................................................................................ 42 I.3.1.5.2. Le stress oxydatif ..................................................................................... 45 I.3.1.5.3. L’activité antioxydante des polyphénols .................................................. 45 I.3.2. Les extractibles des nœuds de bois .......................................................................... 46 I.3.2.1. Teneur et composition des extractibles de nœuds des espèces de Pinus et de Populus .......................................................................................................................... 46 I.3.2.2. Activités des extraits des nœuds ....................................................................... 49 I.3.2.2.1. Inhibition de la peroxydation lipidique et piégeage des radicaux peroxyles .................................................................................................................. 50 I.3.2.3. Activités biocides et antitumorales .............................................................. 51 I.3.2.4. Composition et activité des extraits d’écorces de pin maritime ....................... 52 I.3.2.4.1. Composition des extraits d’écorces de pin maritime................................ 52 1 Sommaire I.3.2.4.2. Activités des extraits d’écorces de pin maritime ...................................... 53 I.3.2.5. Composition et activité des extraits d’écorces de peuplier .............................. 54 I.3.2.5.1. Composition des extraits d’écorces de peuplier ....................................... 54 I.3.2.5.2. Activités des extraits d’écorces de peuplier ............................................. 55 I.3.2.6. Les souches d’arbres ........................................................................................ 55 I.4. L’extraction des polyphénols ......................................................................................... 56 I.4.1. L’extraction à l’eau en continu en extracteur bi-vis ................................................. 58 I.4.1.1. Utilisations de la technologie bi-vis ................................................................. 58 I.4.1.2. Un réacteur thermo-mécanico-chimique .......................................................... 59 I.4.2. L’eau subcritique, une alternative aux solvants d’extraction ................................... 61 I.4.2.1. Les solvants d’extraction solide/liquide ........................................................... 61 I.4.2.2. Les solvants d’extraction des polyphénols ....................................................... 62 I.4.2.3. L’eau subcritique pour l’extraction des polyphénols ....................................... 63 I.5. Conclusion ....................................................................................................................... 67 Chapitre II : Caractérisation des coproduits du bois et extractions en eau subcritique des polyphénols et antioxydants à l’échelle laboratoire ...................................................... 69 II.1. Caractérisation des nœuds, écorces et souches de pin maritime et de peuplier ....... 71 II.1.1. Origine et description des matières premières ......................................................... 71 II.1.2. Conditionnement des matières premières ................................................................ 74 II.1.3. Caractérisation chimique des matières premières .................................................... 75 II.1.3.1. Taux d’extractibles des coproduits de pin maritime et de peuplier .................. 75 II.1.3.2. Teneur en fibres des coproduits de pin maritime et de peuplier ...................... 80 II.1.3.3. Teneur en polyphénols extractibles de coproduits de pin maritime et de peuplier .......................................................................................................................... 82 II.1.4. Activité antiradicalaire des extraits de coproduits de pin maritime et de peuplier
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