La matière grasse laitière anhydre (MGLA) est composée à plus de 98 % de triglycérides. Leur diversité, liée à la nature des acides gras estérifiés, induit un comportement complexe de la MGLA lors de sa cristallisation. Par ailleurs, d’autres composés, dits mineurs, présents de manière endogène ou formés lors de procédés de transformation peuvent moduler le processus de cristallisation. Néanmoins, leurs modes d’action sont encore mal connus, rendant la maitrise du processus de cristallisation délicat. La mise en oeuvre de méthodes de caractérisation à différentes échelles (RMN, diffraction des rayons X, microscopie optique, analyse thermique différentielle, rhéologie) et à différentes températures permet de discriminer les mécanismes d’action des composés mineurs sur la cristallisation de la MGLA en phase continue ou dispersée. Ainsi, les composés mineurs modifient la cinétique de cristallisation de la MGLA, en agissant sur ses deux étapes, la nucléation et la croissance. En accélérant ou en ralentissant la vitesse de cristallisation, ils modifient la nature et/ou la structure du réseau cristallin et, éventuellement, les propriétés macroscopiques de la matière grasse. Les mécanismes d’action des composés mineurs sur la cristallisation de la MGLA dépendent de leur nature chimique (longueur de la chaine carbonée, degré d’insaturation, estérification) et de leur concentration. Lorsque la matière grasse est émulsionnée, son confinement et la création d’interfaces complexifient le processus de cristallisation : les composés mineurs modulent la cristallisation via l’interface ou la phase grasse selon leur affinité préférentielle pour l’une ou l’autre des deux phases de l’émulsion et induisent des propriétés thermiques et structurales spécifiques. Ce travail permet, donc, de mieux comprendre les facteurs qui modulent la cristallisation de la matière grasse et ainsi de mieux maitriser l’un des processus déterminants dans l’élaboration de la structure et de la fonctionnalité des produits laitiers. / Anhydrous Milk Fat (AMF) comprises more than 98% triglycerides. The diversity of the esterified fatty acids induces a complex behavior of AMF during crystallization. In addition, other minor components, either endogenously present or added upon processing modulate AMF crystallization. Nevertheless, the mechanisms underlying their mode of action are still poorly understood, making the mastery of fat crystallization difficult. Several characterization methods (NMR, X-ray diffraction, optical microscopy, differential scanning calorimetry, rheology) were implemented to screen a large set of minor components at different scales and temperatures. The approach enabled to gain knowledge about the involved mechanisms, both in bulk and in the emulsified state. Minor components modify the kinetics of AMF crystallization through their impact on the two main stages of the process, nucleation and growth. By accelerating or slowing down the rate of crystallization, they modify the nature and/or the structure of the crystal lattice and, possibly, the macroscopic properties of AMF. The impact of minor components on AMF crystallization depend on their chemical nature (length of the carbon chain, degree of unsaturation, esterification) and on their concentration. When fat is emulsified, confinement and interfacial effects come into play. Minor components modulate crystallization via the oil/water interface or via the fat phase depending on their preferential solubility, which may induce specific thermal and structural properties. On the whole, this study enables a better understanding of the factors that modulate milk fat crystallization and provides useful guidances for a better control of this key process controlling the structure and function of dairy products.

Submitted by Clebson Anjos (clebson.leandro54@gmail.com) on 2016-03-04T20:58:30Z No. of bitstreams: 1 arquivototal.pdf: 4279867 bytes, checksum: cc6bcf7dbfdbba66c85512e2c1a25a45 (MD5) / Made available in DSpace on 2016-03-04T20:58:31Z (GMT). No. of bitstreams: 1 arquivototal.pdf: 4279867 bytes, checksum: cc6bcf7dbfdbba66c85512e2c1a25a45 (MD5) Previous issue date: 2015-11-27 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / “Manteiga da terra” is a traditional product in the northeast of Brazil that consists of a form of anhydrous cow’s milk fat. This product is susceptible to hydrolytic and oxidative rancidity, responsible for undesirable sensory changes, decreases in nutritional quality and economic impact for the industry. In this study, thermal stability and changes in the physicochemical and sensory profiles were evaluated during storage temperatures of 5, 30, 45 and 60°C at 0, 14, 28, 42 and 56 days. Physicochemical analyses were carried out to evaluate chemical composition and fatty acids profile in the initial time and the storage effects on acidity, peroxide value, TBARS value and objective color. From these results, the activation energy and the induction period were estimated. Microbiological analyses were performed for total and fecal coliforms. Quantitative Descriptive Analysis (QDA) was used to the sensory evaluation of appearance (yellow color, opacity, uniformity and visual viscosity), odor (characteristic of the product and rancid), flavor (characteristic of the product, acid and rancid) and texture (viscosity and granularity). The “manteiga da terra” produced to this study met the standards established by the brazilian legislation with results of 98.96% for fat, 0.07% for moisture, 0.97% for non-fat solids and 0.78% for acidity. The major fatty acids found in the product were oleic (22.66%), palmitic (21.18%) and stearic (13.86%). Saturated fatty acids accounted for 53.72% and unsaturated for 32.24% of the total. There were significant differences for acidity between samples stored at 30, 45 and 60°C, with final values of 0.89, 1.0 and 1.11%, respectively. The peroxide values showed significant increases from 0.50 to 1.30 and 3.99 mEq.kg-1 in samples stored at 45 and 60°C, in this order. The TBARS value was 0.08 mgMDA.kg-1 in the initial time and there were significant increases in the samples stored at 45 and 60°C, with values of 0.12 and 0.19 mgMDA.kg-1, respectively, at the end of 56 days. The parameters L*, a* and b* for objective color characterized the yellow color of the product, with decrease in yellow tone during storage, especially at higher temperatures. The activation energy found for the system was 50.2 kJ.mol-1 and the induction period (in days) was 616 to 5°C, 103 to 30°C, 52 to 45°C and 26 to 60°C. Microbiological analysis indicated the absence of contamination for all samples. In the sensory analysis, the samples kept at 60°C for 56 days had the lowest scores for yellow tone color, opacity, characteristic odor and taste, visual viscosity and viscosity felt at the mouth. On the other hand, they showed a significant increase for the characteristic odor and taste of rancid. The results indicated that the “manteiga da terra” is a stable product for a long period under normal storage conditions. / A manteiga da terra é um produto característico da região nordeste brasileira e consiste de uma forma de gordura anidra proveniente do leite de vaca. Este produto é susceptível às rancificações hidrolítica e oxidativa, responsáveis por alterações sensoriais indesejáveis, diminuição na qualidade nutricional e impacto econômico para a indústria. Neste estudo, foram avaliadas a estabilidade térmica e alterações nos perfis físico-químicos e sensoriais durante o armazenamento em temperaturas de 5, 30, 45 e 60ºC nos tempos 0, 14, 28, 42 e 56 dias. Nas análises físico-químicas, foram realizadas a composição centesimal e o perfil de ácidos graxos no tempo inicial e a avaliação dos efeitos do armazenamento nos parâmetros de acidez, índice de peróxidos, valor de TBARS e cor objetiva. Com estes dados, foram estimados a energia de ativação e o período de indução da amostra. Foram realizadas análises microbiológicas para coliformes a 35 e a 45ºC. A Análise Descritiva Quantitativa (ADQ) foi utilizada na avaliação sensorial dos atributos: aparência (cor amarela, opacidade, homogeneidade e viscosidade visual), odor (característico de manteiga da terra e de ranço), sabor (característico de manteiga da terra, ácido e de ranço) e textura (viscosidade e granulosidade). A manteiga da terra elaborada atendeu aos parâmetros estabelecidos pela legislação com resultados de 98,96% de matéria gorda, 0,07% de umidade, 0,97% de sólidos não gordurosos e 0,78% de acidez. Os ácidos graxos majoritários do produto foram o oleico (22,66%), o palmítico (21,18%) e o esteárico (13,86%). Os ácidos graxos saturados corresponderam a 53,72% e os insaturados a 32,24% do total. No índice de acidez, houve diferença significativa nas amostras armazenadas a 30, 45 e 60ºC, com teores finais de 0,89, 1,01 e 1,11%, respectivamente. Quanto ao índice de peróxidos, inicialmente com 0,50 mEq.kg-1, houve aumentos significativos para as amostras armazenadas a 45 e 60ºC, com índices finais de 1,30 e 3,99 mEq.kg-1, nesta ordem. O valor de TBARS inicial foi de 0,08 mgMDA.kg-1, com aumento significativo nas amostras armazenadas a 45 e 60ºC, com valores de 0,12 e 0,19 mgMDA.kg-1, respectivamente, ao final dos 56 dias. Quanto à cor objetiva, os parâmetros L*, a* e b* caracterizam a cor amarela da amostra que, durante o armazenamento, apresentou um clareamento na tonalidade do amarelo, em especial nas temperaturas mais elevadas. A energia de ativação encontrada para o sistema foi de 50,2 kJ.mol-1 e o período de indução (em dias) foi de 616 para 5ºC, 103 para 30ºC, 52 para 45ºC e de 26 para 60ºC. As análises microbiológicas indicaram ausência de contaminação para todas as amostras. Na análise sensorial, as amostras armazenadas a 60ºC por 56 dias foram as que obtiveram os menores escores para a tonalidade da cor amarela, opacidade, odor e sabor característicos de manteiga da terra, viscosidade visual e viscosidade sentida na boca. Em contrapartida, apresentaram também aumento significativo para o odor e o sabor característicos do ranço. Os resultados do estudo indicaram que a manteiga da terra é um produto que se mantém estável por um longo período, sem alterações importantes antes dos 103 dias de estocagem à temperatura ambiente.