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Le marché des alicaments est en pleine évolution et fait l'objet de recherches importantes dans le secteur agroalimentaire. Cette thèse a pour objectif de caractériser expérimentalement un procédé de production de caramels riches en dianhydrides de fructose (DAF) à l'échelle laboratoire en vue d'une extrapolation à l'échelle semi-pilote par CFD (Computational Fluid Dynamics). Ces caramels ont été préparés à partir d'un sirop de fructose en présence d'une résine qui joue le rôle de catalyseur. L'influence du titre en fructose, de la teneur en résine et de la température a été étudiée. Dans un premier temps, une étude a été menée pour établir des lois de vitesse à partir d'un mécanisme de réaction simplifié. Le suivi cinétique permet d'atteindre jusqu'à 50% de DAF selon les conditions opératoires. Dans un second temps, la caractérisation des fluides prenant part lors de la réaction de caramélisation a été étudiée. Un changement de comportement a été observé lors de la réaction. Le fluide newtonien devient non-newtonien (rhéofluidifiant). Dans un troisième temps, le comportement hydrodynamique du système a été analysé par CFD afin de proposer un semi-pilote présentant des résultats similaires à ceux mesurés à l'échelle laboratoire. La proposition issue du calcul numérique basé sur les nombres adimensionnels est un réacteur discontinu de géométrie cylindrique muni d'un agitateur de type semi-circulaire. Le mélangeur statique a été aussi envisagé. Dans ce cas, la vitesse radiale du fluide (0,2 m.s-1) est le facteur d'extrapolation. Enfin, la faible consommation énergétique de ce réacteur continu présente unvéritable atout pour produire des caramels à l'échelle industrielle. / The functional food market (foods with beneficial properties for health) is increasing and is subject of important research in the food industry. The goal of this thesis has been experimental characterization of caramels with high proportion of di-fructose anhydrides (DFA) processes, using laboratory-scale experiments with the aim to design a semi-pilot-scale reactor by CFD (Computational Fluid Dynamics). These caramels were prepared from a solution of fructose syrup with a resin catalyst. The influence of the ratio fructose/water, proportion of resin and temperature were studied. In a first step, a study was carried out to establish the kinetics laws from a simplified reaction mechanism. The results showed a DAF’s yield of up to 50% depending on the operating conditions. In a second step, the fluids involved in caramelization reaction were characterized. A behavior change outcome was observed during the reaction: the Newtonian fluid becomes non-Newtonian (rheofluidifying). In a third step, the hydrodynamic behavior was analyzed by CFD in order to propose a semi-pilot-scale reactor with similar results to laboratory scale. The numerical modeling based on non-dimensional numbers proposes a batch reactor with cylindrical geometry equipped with a stirrer of semi-circular type. The static mixer was also contemplated. In this case, the radial velocity of fluid (0.2 m.s-1) is the scale up factor. Finally, the low energy consumption of this continuous reactor represents a real advantage to produce caramel to industrial scale / El mercado de los alimentos funcionales (alimentos con propiedades benéficas para la salud) está en plena evolución y ha sidoobjeto de investigación en la industria alimentaria. Esta tesis tiene como objetivo caracterizar experimentalmente un proceso aescala de laboratorio para producir caramelos con alto contenido en dianhídridos de fructosa (DAF), con el fin de extrapolar a unaescala semi-piloto utilizando CFD (Computational Fluid Dynamics). Estos caramelos son obtenidos a partir de jarabe de fructosautilizando una resina como catalizador. Se estudió la influencia de la proporción de fructosa, la proporción de resina y de latemperatura. En una primera etapa, se realizó un estudio para establecer las leyes de velocidad a partir de un mecanismo dereacción simplificado. El seguimiento cinético permitió alcanzar un rendimiento de hasta 50% en DAF dependiendo de lascondiciones operatorias. En una segunda etapa, se realizó una caracterización de los fluidos implicados en la reacción decaramelización. Un cambio en el comportamiento del fluido durante la reacción fue observado. El fluido newtoniano se comportacomo fluido no-newtoniano (adelgazante). En una tercera etapa, el comportamiento hidrodinámico del sistema fue analizadomediante CFD, a fin de proponer un reactor semi-piloto que presente resultados similares a los calculados para la escalalaboratorio. La propuesta resultante del modelo matemático basado en los números adimensionales, es un reactor por lotes con unageometría cilíndrica y un agitador de tipo semicircular. Un mezclado estático fue también conceptualizado. En este caso, lavelocidad radial del fluido (0,2 m.s-1) fue el factor de extrapolación del proceso. Por último, el bajo consumo de energía de estereactor continuo representa una verdadera ventaja para la producción de caramelos a nivel industrial.

Doctor of Philosophy / Food Science Institute / J. Scott Smith / The International Agency for Research on Cancer (IARC) has classified 4(5)-methylimidazole (4-MeI) as a possible human carcinogen. Also, the National Toxicology Program (NTP) has concluded that 4-MeI is a probable cancer causing agent. Even though 4-MeI has been detected in several processed foods no research has been conducted to measure levels of 4-MeI in processed meat. A method using isobutylchloroformate (IBCF) and gas chromatography mass-spectrometry (GC-MS) was developed to detect and quantify 4-MeI in processed meat products. Levels of 4-MeI ranged from 0.04 to 1.01 μg/g with recovery of 94.76 to 103.94%. Formation of 4-MeI in glucose-amino acid model system was studied. [subscript]D-Glucose (Glu) was mixed individually in equimolar concentrations of 0.05, 0.1, or 0.15 M and equal volume with [subscript]L-Alanine (Ala), [subscript]L-Arginine (Arg), Glycine (Gly), [subscript]L-Lysine (Lys), and [subscript]L-Serine (Ser); and the mixtures were heat treated at 60, 120, and 160°C for 1 h. Among all tested amino acids, Glu-Arg produced the highest level of 4-MeI. The Glu-Lys model system showed higher browning and lower concentrations of 4-MeI. The effect of ascorbic acid (ASA), a strong antioxidant, was studied in the Glu-Arg model system. Four concentrations of ASA (0.0375, 0.075, 0.15, and 0.3 M) were mixed with 0.15 M equimolar of Glu-Arg and heat treated at 160°C for 1h. ASA inhibited formation of 4-MeI by 40.29, 69.94, 75.13, and 96.25% for the 0.0375, 0.075, 0.15, and 0.3 M concentrations. Contrarily, ascorbic acids increased the browning in all treatments compared to control treatment by 10.67, 15.47, 18.4, and 28.8% for the 0.0375, 0.075, 0.15, and 0.3 M concentrations. Adding ASA to processed food may reduce formation of 4-MeI and increase the browning that is a desired attribute to processed meat products.

Caramel is a mixture of sugars, milk proteins, fat and water cooked at high temperatures to initiate Maillard reactions. We study caramels as ‘active emulsion-filled protein gels’, in which fat droplets are chemically-bonded to a background gel matrix of cross-linked proteins in a concentrated aqueous sugar solution. A ‘caramel region’ in composition space is delimited by the varying the four ingredients; sugar, milk protein, fat and water. The boundaries of the composition space define various modes of ‘failure’. Boundaries are determined for transitions to toffee and emulsification failure leaking out of the caramel, and protocol dependent failures, scum formation during the cooking step and subsequent boil over or the formation of a ‘creme Chantilly. Oscillatory rheology within the caramel region reveals that we can superpose the mechanical spectra of all caramels into a single pair of G'(ω),G''(ω) master curves using time-composition superposition (tCS) over 12 decades of frequency, so that all caramels are instances of an underlying ‘universal material’. The master curve is an example of a very lightly cross-linked amorphous polymer, a weak rubber. Utilising the cross-over point of G'(ω) and G''(ω) as a common point to compare caramel master curves the viscous and elastic dependency of caramel is determined and linked to the caramels ingredients. Viscosity is dependent on the aqueous sugar content and the elastic dependency on protein content. This insight constrains the molecular mechanisms for structure formation, and implies that measuring a couple of parameters suffices to predict the rheology of caramels over 12 orders of magnitude in frequency.

Studien ämnar analysera hur filmen Caramel bryter stereotyper genom de fem huvudkaraktärerna och hur regissören Nadine Labaki använder medieaktivism för att förändra bilden av arabiska kvinnor på film. Detta har genomförts genom en kvalitativ semiotisk analys där begreppen denotation och konnotation applicerats som metod. Mitt teoretiska ramverk har utgjorts av begreppen representation, koder, symboler, stereotyper, feministisk filmteori och medieaktivism. Fem utvalda karaktärer har analyserats baserat på deras representation i filmen. Resultatet av studien visar att Caramel har brutit några stereotyper av arabiska kvinnor i filmen och att Nadine Labaki använt feminism och aktivism för att ändra representationen av arabiska kvinnor i film. / The study intends to analyze how the film Caramel breaks stereotypes through the five main characters and how director Nadine Labaki uses media activism to change the image of Arab women in film. This has been carried out through a qualitative semiotic analysis where the concepts of denotation and connotation have been applied as a method. My theoretical framework has been made up of the concepts of representation, codes, symbols, stereotypes, Feminist film theory and media activism. Five selected characters have been analyzed based on their representation in the film. The result of the study shows that Caramel has broken some stereotypes of Arab women in the film and that Nadine Labaki used feminism and activism to change the representation of Arab women in film.

Master of Science / Food Science Institute - Animal Science & Industry / Fadi M. Aramouni / Smoke flavored foods continue to be a popular choice among consumers. In this study, a caramel-type flavor in whipped cream applications via Maillard reaction pathways was evaluated. A highly refined liquid smoke fraction was developed using a delignified pulp wood source, and a patented activated carbon filtration process. To maximize sensory and reactionary capabilities, a liquid smoke fraction with phenol and carbonyl concentrations of 0.07mg/ml and 12.9g/100ml, respectively, was developed. Heavy cream containing a 0.075% addition of the refined liquid smoke fraction was evaluated when reacted at 50, 63, and 72°C for 15 sec prior to chilling at 0°C for 12 h, and whipping for 8 min using a handheld mixer. Sensory analysis showed the addition of liquid smoke increased whipped cream sweetness and caramel flavors, while imparting minimal off-flavors. Probable Maillard pathways were predicted for the reaction taking place between the liquid smoke and the dairy proteins upon thermal processing. This technology can be used to develop other foods which are not traditionally smoke flavored.

Leung Bo-Shan. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2001. / Includes bibliographical references (leaves 148-159). / Abstracts in English and Chinese. / Abstract --- p.i / Acknowledgements --- p.v / List of Abbreviations --- p.vi / List of Tables --- p.viii / List of Figures --- p.ix / Chapter 1 --- Introduction / Chapter 1.1 --- Food colorants --- p.1 / Chapter 1.2 --- Caramel --- p.3 / Chapter 1.2.1 --- Classes of caramel --- p.3 / Chapter 1.2.2 --- Toxicological studies of caramel --- p.5 / Chapter 1.3 --- Castanea mollissima --- p.9 / Chapter 1.4 --- Antioxidants --- p.10 / Chapter 1.4.1 --- Background --- p.10 / Chapter 1.4.2 --- Methods used to evaluate the antioxidative activity --- p.12 / Chapter 1.4.2.1 --- DPPH* scavenging method --- p.13 / Chapter 1.4.2.2 --- High performance liquid chromatography (HPLC) --- p.13 / Chapter 1.5 --- Microtox® test --- p.19 / Chapter 1.6 --- Mutatox® test --- p.19 / Chapter 1.7 --- Methods used to evaluate the functions of major organs --- p.20 / Chapter 1.7.1 --- Liver --- p.20 / Chapter 1.7.2 --- Kidneys --- p.23 / Chapter 1.8 --- Toxicology --- p.25 / Chapter 1.8.1 --- Acute toxicity test --- p.25 / Chapter 1.8.2 --- Chronic toxicity test --- p.26 / Chapter 1.9 --- Objective --- p.27 / Chapter 2 --- Materials and Methods --- p.28 / Chapter 2.1 --- Plant materials --- p.28 / Chapter 2.2 --- Sample preparation --- p.28 / Chapter 2.3 --- Pigment characterization --- p.30 / Chapter 2.3.1 --- Stability test --- p.30 / Chapter 2.3.2 --- HPLC separation of CP --- p.31 / Chapter 2.3.3 --- Determination of antioxidative activity with the DPPH* scavenging method --- p.31 / Chapter 2.4 --- Microtox® test --- p.33 / Chapter 2.5 --- Mutatox® test --- p.34 / Chapter 2.6 --- Acute toxicity test --- p.35 / Chapter 2.6.1 --- Animals --- p.35 / Chapter 2.6.2 --- Housing and maintenance --- p.35 / Chapter 2.6.3 --- Experimental design --- p.37 / Chapter 2.6.4 --- Chemicals --- p.39 / Chapter 2.6.5 --- Clinical pathology test --- p.41 / Chapter 2.6.5.1 --- Haematology --- p.41 / Chapter 2.6.5.2 --- Blood chemistry --- p.45 / Chapter 2.6.5.3 --- Urinalysis --- p.55 / Chapter 2.6.6 --- Histological study --- p.57 / Chapter 2.6.7 --- Statistical analysis --- p.57 / Chapter 2.7 --- Chronic toxicity test --- p.59 / Chapter 2.7.1 --- Animals --- p.59 / Chapter 2.7.2 --- Housing and maintenance --- p.59 / Chapter 2.7.3 --- Experimental design --- p.59 / Chapter 2.7.4 --- Chemicals --- p.60 / Chapter 2.7.5 --- Clinical pathology test --- p.61 / Chapter 2.7.5.1 --- Haematology --- p.61 / Chapter 2.7.5.2 --- Blood chemistry --- p.62 / Chapter 2.7.5.3 --- Urinalysis --- p.62 / Chapter 2.7.6 --- Histological study --- p.62 / Chapter 2.7.7 --- Statistical analysis --- p.62 / Chapter 3 --- Results --- p.63 / Chapter 3.1 --- Pigment characterization --- p.63 / Chapter 3.1.1 --- Stability test --- p.63 / Chapter 3.1.2 --- HPLC separation of CP --- p.63 / Chapter 3.1.3 --- Antioxidative activities of CP preparations --- p.63 / Chapter 3.2 --- Microtox® test --- p.65 / Chapter 3.3 --- Mutatox® test --- p.65 / Chapter 3.4 --- Acute toxicity test --- p.66 / Chapter 3.4.1 --- Growth rate --- p.66 / Chapter 3.4.2 --- Food and fluid consumption --- p.66 / Chapter 3.4.3 --- Organ-weight --- p.66 / Chapter 3.4.4 --- Clinical pathology tests --- p.68 / Chapter 3.4.4.1 --- Haematology --- p.68 / Chapter 3.4.4.2 --- Blood chemistry --- p.70 / Chapter 3.4.4.3 --- Urinalysis --- p.76 / Chapter 3.4.5 --- Histological study --- p.76 / Chapter 3.5 --- Chronic toxicity test --- p.77 / Chapter 3.5.1 --- Growth rate --- p.77 / Chapter 3.5.2 --- Food and fluid consumption --- p.77 / Chapter 3.5.3 --- Organ-weight --- p.77 / Chapter 3.5.4 --- Clinical pathology tests --- p.78 / Chapter 3.5.4.1 --- Haematology --- p.78 / Chapter 3.5.4.2 --- Blood chemistry --- p.80 / Chapter 3.5.4.3 --- Urinalysis --- p.82 / Chapter 3.5.5 --- Histological study --- p.82 / Chapter 4 --- Discussion --- p.137 / Chapter 4.1 --- Pigment characterization --- p.137 / Chapter 4.2 --- Toxicological studies of CP --- p.140 / Chapter 5 --- Conclusion --- p.147 / References --- p.148

L’objectif de cette étude est d’étudier l’impact de la fraction volatile odorante et de la fraction non-volatile sur la perception de la flaveur du caramel. Dans la première étape, la fraction volatile du caramel a été analysée par Chromatographie en Phase Gazeuse couplée à l’Olfactométrie (GC/O), par GC couplée à la Spectrométrie de Masse (GC/MS) et par heart-cutting MDGC. Les résultats mettent en évidence une centaine de composés volatils et démontrent la richesse aromatique du caramel. L’objectif de la deuxième étape était d’évaluer la contribution de ces composes volatils à la typicité odorante du caramel. Des études ont montré que l’intensité odorante n’était pas suffisante pour évaluer l’impact des composés. Ce travail de thèse propose une approche originale de recombinaison d’odeur à partir de composés triés selon leur qualité odorante. Les résultats montrent que la typicité odorante caramel est le fruit d’un équilibre entre les notes caramel, fruité, fruits secs, végétal, animal, grillé, floral et piquant. Des tests d’addition, d’omission et d’un plan d’expérience factoriel complet ont démontré l’existence d’interactions perceptives. L’objectif de la dernière étape était d’étudier l’impact de la fraction non volatile sur la perception de la flaveur du caramel. L’étude de la libération de composés d’arôme in vitro par analyses SPME/GC/MS dans différentes matrices non volatiles démontre l’existence d’interactions physico-chimiques entre les composés d’arôme et les macromolécules non volatiles. Ces premiers résultats laissent supposer que la fraction non volatile est susceptible de moduler la perception de la flaveur / The aim of this study was to investigate the impact of the volatile odorant fraction and the non-volatile matrix on the perception of the caramel flavour. The first step focused on the analytical characterization of the volatile odorant fraction of aromatic caramel thanks to Gas Chromatography coupled to Olfactometry (GC/O), GC/Mass Spectrometry (GC/MS) and heart-cutting MDGC/MS/O. Results highlighted the presence of more than one hundred compounds and demonstrated the complexity of the caramel volatile fraction. The objective of the second step was to understand the contribution of odorant compounds identified to the caramel aroma typicality. Literature shows that odour intensity is not sufficient to evaluate the impact of compounds on the aroma. This thesis proposed an original approach to carry out the aroma recombination by taking into account odour qualities. Results showed that the caramel typicality results from a complex balance between caramel, fruity, vegetal, sharp, nutty, floral, roasted and animal odours. Omission, addition tests and a 24 factorial design showed the existence of perceptive interactions. The third step focused on studying the impact the macromolecules that constitute the non-volatile fraction on the perception of caramel flavour. In vitro aroma release was followed by SPME/GC/MS in different matrices varying in non-volatile composition. Results evidence physico-chemical interactions between aroma and macromolecule of the non-volatile fraction. Those preliminary results suggest that the non-volatile matrix is able to impact the flavour perception

Le caramel liquide, obtenu par le traitement thermique des sucres, est couramment utilisé pour modifier le goût ou la couleur des produits agroalimentaires.Parmi les promoteurs de caramélisation autorisés, l’ammoniaque (pour les caramels colorants de classe III) et les sels d’ammonium (pour ceux de classe IV) sont source de composés néoformés indésirables (CNI) comme le 2-acétyl-4-(1,2,3,4-tétrahydroxybutyl)imidazole (THI), immunosuppresseur, et le 4-méthylimidazole (4MeI), agent convulsif. Ces molécules ont des teneurs limitées par la réglementation Européenne à 10 et 250 ppm respectivement. Pour améliorer la connaissance de la chimie du caramel et la qualité des caramels colorants en contrôlant la formation des CNI, il est nécessaire de développer des méthodes analytiques fiables, rapides et faciles à mettre en œuvre. Ce travail de thèse présente le développement de nouvelles méthodes basées sur la chromatographie en phase liquide à deux-dimensions (LC-LC). Ces méthodes très sélectives permettent de minimiser le temps d’analyse puisque la préparation de l’échantillon se réduit à une simple dilution dans l’eau et les deux séparations chromatographiques en cascade sont réalisées sur un système totalement automatisé. La validation des méthodes par les profils d’exactitude a permis d’assurer que 90 % des résultats sont à moins de 20 % de la valeur vraie dans le domaine de concentration 10 à 50 ppm pour le THI, 20 à 500 ppm pour le 4MeI, 200 à 2500 ppm pour le fructose, saccharose, lactose, maltose et maltotriose et 500 à 2500 ppm pour le glucose.Ces méthodes sont enfin appliquées au suivi de la réaction de caramélisation et au contrôle qualité des produits finis. / Caramel liquid, obtained by heat treatment of sugars, is commonly used to alter the taste or colour of food products.Among promoters of caramelization allowed, ammonia (for caramel colours of class III) and ammonium salts (for those of class IV) are a source of neoformed contaminants (NFC) such as 2-acetyl-4-(1,2,3,4-tetrahydroxybutyl)imidazole (THI), immunosuppressive agent, and 4-methylimidazole (4MeI), convulsive agent. These molecules have contents limited by the European regulations to 10 and 250 ppm, respectively.To improve knowledge of the chemistry of caramel and quality of caramel colours by controlling the formation of NFC, it is necessary to develop analytical methods that are both reliable, fast and easy to implement. This thesis presents the development and validation of new methods based on two-dimensional liquid chromatography (LC-LC). These very selective methods can minimize analysis time since sample preparation is reduced to a simple dilution with water and the two consecutive chromatographic separations are performed on a fully automated system. The method validation by the accuracy profiles allowed to show that 90 % of obtained results correspond to the agreement value more or less 20 %, in the field of concentration 10 to 50 ppm for THI, 20 to 500 ppm for 4MeI, 200 to 2500 ppm for fructose, sucrose, lactose, maltose and maltotriose and 500 to 2500 ppm for glucose.These methods are finally applied to monitor the reaction of caramelization and to control the quality of finished products.