Etude de l'influence du traitement thermique sur la qualité et la composition des huiles végétales: les apports des méthodes chimiométriques.

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Rana, Cheikhousman (2006) Etude de l'influence du traitement thermique sur la qualité et la composition des huiles végétales: les apports des méthodes chimiométriques. Doctorat Chimie analytique, Chimie analytique, INAPG 2006INAP0005.

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Table des Matières

Abréviations 5
Tables des illustrations 6
Introduction 19
Partie I: Bibliographie
1. Huiles végétales 25
1.1. Les lipides 25
1.2. Huile d'olive 28
1.2.1. Huile d'olive - définition 28
1.2.1.1. L'Accord International des Huiles d'Olive et des Olives de Table 29
1.2.2. Production 29
1.2.3. Consommation 30
1.2.4. Composition chimique et caractéristiques organoleptiques de l'huile d'olive 31
1.2.4.1. Acides gras et triacylglycérols 32
1.2.4.2. Constituants mineurs 33
1.2.5. Critères de qualité 40
1.3. Huile de colza 42
1.3.1. Composition chimique et étude organoleptique de l'huile de colza 43
1.3.1.1. Développement des variétés et des types de l'huile de colza 43
2. Généralités sur les mécanismes de dégradations des huiles 49
2.1. Introduction 49
2.2. Phénomène d'oxydation 49
2.2.1. Productions d'espèces radicalaires 49
2.2.2. Formations des produits secondaires d'oxydation 51
2.2.3. Terminaison 52
2.3. Nature et mode d'action des antioxydants 53
2.3.1. Les antioxydants phénoliques 54
2.3.2. Tocophérols 55
2.3.3. Oxydation et réaction en chaîne 57
3. Spectroscopie de fluorescence 59
3.1. Principe 59
3.2. Fluorescence des huiles alimentaires 59
3.3. Fluorescence des produits de peroxydation 60
3.4. Application de la spectroscopie de fluorescence à l'étude des huiles 61
4. Spectroscopie Infrarouge 62
4.1. Spectroscopie Proche Infrarouge 62
4.1.1. Applications des spectres PIR 63
4.2. Spectroscopie Moyen Infrarouge 64
4.2.1. Principes de base 65
4.2.1.1. Interféromètres 65
4.2.1.2. Spectroscopie infrarouge quantitative 67
24.2.1.3. Réflexion Totale Atténuée ATR ("Attenuated Total Reflectance") 67
4.2.2. Origine des positions et des intensités des pics en infrarouge 70
4.2.2.1. Positions des pics 70
4.2.2.2. Origine de l'intensité des pics 73
4.2.2.3. Origine des plages de nombres d'onde caractéristiques 73
4.2.3. Application de la spectroscopie moyen infrarouge à l'étude des huiles - 74
4.2.3.1. Etude du degré d'insaturation des lipides 74
4.2.3.2. Etude de la longueur de chaîne des lipides 75
4.2.3.3. Dosage des lipides 75
4.2.4. Attribution des bandes d'absorption des lipides dans le moyen infrarouge 76
Partie II: Matériel et Méthodes
5. Méthodes analytiques 78
5.1. Spectroscopie de fluorescence 78
5.1.1. Conditions de chauffage 78
5.1.2. Methodes chimiques 79
5.1.2.1. Dosages des hydroperoxydes 79
5.1.2.2. Dosages de vitamine E (-tocophérol) 79
5.1.2.3. Dosage des composés phénoliques 80
5.1.2.4. Spectres de fluorescence 81
5.2. Spectroscopie moyen Infrarouge (MIR) 82
5.2.1. Appareillage 82
5.2.2. Modes d'acquisition 83
5.2.3. Paramètres de la méthode 84
5.2.3.1. Paramètres optiques 84
5.2.3.2. Paramètres d'acquisition 84
5.2.4. Echantillons 85
5.2.4.1. Acides gras de références 85
5.2.4.2. Huiles végétales 86
6. Méthodes chimiométriques appliquées 87
6.1. Prétraitements des données spectrales 87
6.1.1. Amélioration du signal 88
6.1.2. Sélection de variables 91
6.2. Méthodes exploratoires 91
6.3. Méthodes prédictives 94
6.3.1. Validation Croisée ("Cross-Validation") 96
6.3.2. Critère de Durbin-Watson 96
Partie III: Résultats et Discussions
7. Spectroscopie de fluorescence 99
7.1. Introduction 99
7.2. Huile d'olive extra vierge chauffée à 170 °C (OEV-170) 99
7.2.1. Evolution des composés phénoliques et de la vitamine E 99
7.2.1.1. Par spectroscopie de fluorescence 99
7.2.1.2. Par HPLC 102
7.2.1.3. Comparaison les résultats obtenus par spectroscopie de fluorescence et HPLC pour la vitamine E et les composés phénoliques 104
7.2.1.4. Analyse en Composantes Principales (ACP) 105
7.2.1.5. Régression au sens des moindres carrés partiels (PLS) 107
37.2.2. Evolution des hydroperoxydes pendant le chauffage 109
7.2.2.1. Par la méthode colorimétrique indirecte 109
7.2.2.2. Par spectroscopie de fluorescence 109
7.2.2.3. Comparaison les résultats obtenus par spectroscopie de fluorescence et la méthode colorimétrique pour les hydroperoxydes - 111
7.2.2.4. Analyse en Composantes Principales (ACP) 111
7.2.2.5. Régression au sens des moindres carrés partiels (PLS) 113
7.3. Huile d'olive extra vierge chauffée à 190 °C (OEV-190) 114
7.3.1. Evolution de la vitamine E pendant le chauffage 114
7.3.1.1. Par HPLC 114
7.3.1.2. Par la spectroscopie de fluorescence 115
7.3.1.3. Comparaison entre les résultats obtenus par la spectroscopie de fluorescence et
HPLC pour la vitamine E 118
7.3.1.4. Analyse en Composantes Principales (ACP) 118
7.3.1.5. Régression au sens des moindres carrés partiels (PLS) 120
7.3.2. Evolution des hydroperoxydes pendant le chauffage 121
7.3.2.1. Par la méthode colorimétriques indirecte 121
7.3.2.2. Par spectroscopie de fluorescence 122
7.3.2.3. Comparaison les résultats obtenus par la spectroscopie de fluorescence et la méthode colorimétrique pour l'hydroperoxydes 123
7.3.2.4. Analyse en Composantes Principales (ACP) 124
7.3.2.5. Régression au sens des moindres carrés partiels (PLS) 126
7.4. Conclusion 127
8. Spectroscopie Moyen InfraRouge (MIR) 129
8.1. Introduction 129
8.2. Etude des spectres Moyen InfraRouge (MIR) d'acides gras 129
8.2.1. Analyse en Composantes Principales (ACP) des acides gras libres en MIR sur ATR
"Golden Gate" 132
9. Evolution des spectres MIR des huiles au cours du chauffage 137
9.1. Huile d'olive extra vierge chauffée à 170 °C (OEV-170) 137
9.1.1. Evolution des spectres de l'huile (OEV-170) au cours du chauffage 138
9.1.2. Analyse en Composantes Principales (ACP) 147
9.1.3. Analyse en Composantes Indépendantes (ICA) 151
9.2. Huile d'olive extra vierge chauffée à 190 °C (OEV-190) 155
9.2.1. Evolution des spectres de l'huile (OEV-190) au cours du chauffage 156
9.2.2. Analyse en Composantes Principales (ACP) 162
9.2.3. Analyse en Composantes Indépendantes (ICA) 164
9.3. Huile de colza chauffée à 170 °C (C-170) 167
9.3.1. Evolution des spectres de l'huile (C-170) au cours du chauffage 168
9.3.2. Analyses en Composantes Indépendantes (ICA) 172
9.4. Huile de colza chauffée à 190 °C (C-190) 177
9.4.1. Evolution des spectres de l'huile (C-190) au cours du chauffage 178
9.4.2. Analyse en Composantes Indépendantes (ICA) 182
9.5. Mélange 50/50 d'huile d'olive extra vierge et d'huile de colza chauffé à 170 °C (HOC-170) et à 190 °C (HOC-190) 186
9.5.1. Evolution des spectres des mélange (HOC-170) et (HOC-190) au cours du chauffage
1869.5.2. Analyses en Composantes Indépendantes "ICA" pour le mélange (HOC-170)
1929.5.3. Analyse en Composantes Indépendantes "ICA" pour le mélange (HOC-190)
195410. Comparaison du comportement des huiles en fonction de chauffage 199
10.1. Une huile chauffée à deux températures différentes (170 °C et 190 °C) 199
10.1.1. Huile d'olive 199
10.1.1.1. Comparaison de l'ICA avec l'ACP de l'huile (OEV-170) 203
10.1.1.2. Comparaison de l'ICA avec l'ACP de l'huile (OEV-190) 203
10.1.1.3. Comparaison entre l'ICA de l'huile d'olive extra vierge chauffée à 190 °C et à
170 °C 204
10.1.2. Huile de colza 205
10.1.2.1. Comparaison d'ICA de l'huile (C-190) (ICAC190) avec l'ICAC170 et l'ICAO190
20810.1.3. Huile de mélange (50 % huile d'olive extra vierge et 50 % huile de colza) (HOC)
20910.1.3.1. Comparaison d'ICA du mélange (HOC-190) avec le mélange (HOC-170) 212
10.2. Différentes huiles (C, OEV, HOC) chauffée à la même températures 213
10.2.1. Chauffage à 170 °C 213
10.2.1.1. Comparaison d'ICA du mélange (HOC-170) avec l'huile (C-170) et l'huile
(OEV-170) 217
10.2.2. Chauffage à 190 °C 218
10.2.2.1. Comparaison d'ICA du mélange (HOC-190) avec l'huile (C-190) et l'huile
(OEV-190) 221
11. Régression au sens des moindres carrés Partiels (PLS) 224
11.1. Régression basée sur le spectre entier 224
11.1.1. Huile d'olive extra vierge chauffée à 170 °C 226
11.1.2. Huile d'olive extra vierge chauffée à 190 °C 229
11.1.3. Huile de colza chauffée à 170 °C 231
11.1.4. Huile de colza chauffée à 190 °C 233
11.1.5. Huile de mélange chauffée à 170 °C (HOC-170) 235
11.1.6. Huile de mélange chauffée à 190 °C (HOC-190) 236
11.2. Régression basée sur des régions spectrales 238
11.3. Conclusion 241
Conclusion générale 243
Références bibliographiques 246
Annexe

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