This diploma thesis is focused on determining the physico-chemical stability of toothpastes. It is divided into theoretical and practical part. The theoretical part of the work deals with toothpastes, their short history and composition. Stability studies and methods of stability analysis are described below. In the practical part were performed long-term and accelerated stability studies on anhydrous toothpastes, on water-based toothpastes and on toothpastes based on sodium bicarbonate. The physical stability of the products was evaluated by monitoring the appearance and color visually and odor sensory, the pH value using a pH meter and the viscosity with a rotational viscometer. Chemical stability was monitored by determining the free fluorine content by ion chromatography and by ion-selective electrode, total phosphates and potassium also by ion chromatography, sodium bicarbonate by titration, soluble zinc by atomic absorption spectrometry and water activity was also monitored.

Pharmaceutical solids tend to exist in different physical forms termed as polymorphs. Issues about pharmaceutical systems are mainly concerned with the active ingredient's physico-chemical stability and bioavailability. The main aim of this study is to investigate the non-bonded interactions in pharmaceutical solids that govern the physical pharmaceutics performance of such materials and through the use of structural techniques and correlation of these results with crystal structural database to establish the presence of physical motifs in selected systems. Structural motifs were identified by the use of single crystal and crystal packing analysis on diverse range of pharma-relevant materials including chalcones, cryptolepines, biguanides and xanthines. These selected systems were validated using functional group and molecular analysis and correlating them to the Cambridge Structural Database. Crystallization studies are done on these selected systems as well as exploiting those using synthetic analogues. A total of 51 crystal structures were investigated including 16 new structure determinations. Addition synthesis of new xanthines to investigate novel intermolecular patterns was also undertaken. The understanding and exploitation of intermolecular interactions involving hydrogen bonds and coordination complexation during packing can be used in the design and synthesis of solid state molecular structures with desired physical and chemical properties.

Pharmaceutical solids tend to exist in different physical forms termed as polymorphs. Issues about pharmaceutical systems are mainly concerned with the active ingredient's physico-chemical stability and bioavailability. The main aim of this study is to investigate the non-bonded interactions in pharmaceutical solids that govern the physical pharmaceutics performance of such materials and through the use of structural techniques and correlation of these results with crystal structural database to establish the presence of physical motifs in selected systems. Structural motifs were identified by the use of single crystal and crystal packing analysis on diverse range of pharma-relevant materials including chalcones, cryptolepines, biguanides and xanthines. These selected systems were validated using functional group and molecular analysis and correlating them to the Cambridge Structural Database. Crystallization studies are done on these selected systems as well as exploiting those using synthetic analogues. A total of 51 crystal structures were investigated including 16 new structure determinations. Addition synthesis of new xanthines to investigate novel intermolecular patterns was also undertaken. The understanding and exploitation of intermolecular interactions involving hydrogen bonds and coordination complexation during packing can be used in the design and synthesis of solid state molecular structures with desired physical and chemical properties.

Dans le cadre du dragage de Port-Camargue (projet national ECODREDGE-MED), l'objectif principal des travaux de thèse a été d'étudier la re-sédimentation des sédiments ré-immergés et d'appréhender les transferts de matière (particulaires et moléculaires) associés. Une approche expérimentale de caractérisation a été réalisée pour appréhender ces phénomènes, aux échelles macroscopiques (mécanismes de sédimentation), mésoscopiques (transferts de matière particulaires) et moléculaires (phénomènes de sorption). Les travaux ont porté sur l'étude de cinq sédiments et de leurs fractions granulométriques. Une méthode de séparation granulaire a donc été développée et optimisée en ce sens, soulignant l'importance de vérifier la qualité de la séparation lorsque les développements portent sur les fractions granulaires. L'approche morpho-granulaire utilisée dans la caractérisation de ces systèmes a permis, dans un premier temps, de mettre en évidence le comportement cohésif des sédiments et d'identifier différents types d'agglomérats. Elle a ensuite été utilisée pour proposer une méthode de classification simple et rapide des sédiments, basée essentiellement sur la détermination, par granulométrie laser, du rapport volumique limon/sable.En second lieu, le comportement à la re-sédimentation a été appréhendé en étudiant la stabilité physico-chimique des particules dans la colonne de sédimentation grâce à un analyseur de suspensions concentrées, le Turbiscan MA2000. Cette stratégie apporte de nouvelles connaissances, notamment sur les mécanismes de sédimentation et l'impact de certains paramètres comme le rapport limon/sable, la salinité ou la fraction volumique sur ces mécanismes. Combinée à l'analyse du Carbone Organique Total (COT), des transferts de matière ont été identifiés dans la colonne de sédimentation, via les phénomènes interparticulaires (agglomération/dispersion) et les phénomènes de sorption (adsorption/désorption). / In the framework of Port-Camargue dredge (ECODREDGE-MED project), the main objective was to study the dredged sediment re-sedimentation and matter transfers (particular and molecular matter). An experimental characterization approach was realized in order to study these phenomena working at different scales : macroscopic (sedimentation mechanisms), mesoscopic (particular matter mobilization) and molecular (sorption phenomena). These research works focused on study of five sediments and their granular fractions. A dispersion granular method was developed and highlighted the importance to verify dispersion quality of processes concerning study of granular fractions. Morpho-granular approach used in theses works permitted to highlight cohesive aspect of sediments and to identify different agglomerate types. This approach was also used to propose a classification method of sediments, based on limon/sand ratio determination by laser granulometry.Secondly, re-sedimentation behavior was investigated studying physico-chemical stability of particles in the water column with a suspension analyszer (Turbiscan MA2000). The results contributed knowledge on sedimentation mechanisms and parameter (limon/sand ratio, salinity and volume fraction) influence. With the use of TOC analyze (Total Organic Carbone), matter transfers were identified in water column, via interparticular phenomena (agglomeration/dispersion) and sorption phenomena (adsorption/désorption).

CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior / O caju destaca-se dentre as espÃcies frutÃferas nativas do Nordeste, por possuir elevada potencialidade para o consumo in natura e processamento industrial. A polpa e o suco sÃo importantes componentes da dieta humana por serem considerados uma fonte natural de carboidratos, carotenoides, vitaminas e compostos fenÃlicos, substÃncias com alto potencial antioxidante, e tÃm despertado o interesse de diferentes grupos de pesquisa. Este trabalho teve como objetivo estudar a estabilidade da polpa de caju com conservantes, pasteurizada e concentrada congelada durante 12 meses de armazenamento, atravÃs de determinaÃÃes quÃmicas, fÃsico-quÃmicas e microbiolÃgicas e a elaboraÃÃo de nÃctar e suco tropical adoÃado, estudando a estabilidade sensorial dos mesmos durante 360 dias de armazenamento da polpa. As polpas nÃo apresentaram interaÃÃo significativa para pH, sÃlidos solÃveis, acidez titulÃvel e coordenada de cor a. O pH e os sÃlidos solÃveis variaram com o tempo mas mantiveram-se dentro dos padrÃes da legislaÃÃo. A acidez nÃo variou com o armazenamento. A coordenada de cor a* ajustaram ao modelo cÃbico. O Ãcido ascÃrbico variou de 190,65 a 308,45mg/100g na polpa com conservantes, 170,95 a 299,70 mg/100g na polpa pasteurizada e de 514,68 a 865,42mg/100g na polpa concentrada, valores estes bastante expressivos. Pigmentos escuros solÃveis, luminosidade, hue, croma, carotenoides, teor de polpa, aÃÃcares totais apresentaram interaÃÃo significativa e foram avaliados por regressÃo variando com o tempo de armazenamento, exceto a coordenada de cor b*. Os teores de aÃÃcares totais mantiveram-se em torno de 10,01 a 13,25% nas polpas com conservantes e pasteurizadas a 24 a 27% na polpa concentrada, sendo estes em sua maioria representados por aÃÃcares redutores. As anÃlises microbiolÃgicas confirmaram a eficÃcia das etapas de processamento, tratamento tÃrmico e concentraÃÃo na manutenÃÃo da qualidade microbiolÃgica, uma vez que nÃo foi observado crescimento de microrganismos durante o perÃodo de armazenamento. Os nÃctares e os sucos tropicais adoÃados de caju apresentam-se na faixa de aceitaÃÃo sensorial em todos os atributos avaliados. O congelamento das polpas de caju com conservantes, pasteurizada e concentrada à viÃvel uma vez que nÃo ocorrem perdas significativas na qualidade dos produtos. A polpa de caju concentrada apresentou as melhores notas nos atributos sensoriais avaliados. / The cashew (Anacardium occidentale, L.) has a great economic importance to the Northeast region, notably for the great acceptance by consumers, both for their sensory properties (color, aroma, flavor, texture) as for its nutritional and functional values. It stands out among the fruit species native to the Northeast because it has high potential for fresh consumption and industrial processing. The cashew and cashew apple juice are important components of the human diet because they are considered a natural source of carbohydrates, carotenoids, vitamins and phenolic compounds, substances with high antioxidant potential, and have attracted the interest of various research groups. This work aimed to study the stability of cashew apple pulp with preservatives, pasteurized and concentrated frozen storage for 12 months, through to chemical, physical-chemical and microbiological analysis. And production of cashew apple nectar and cashew apple sweetened tropical juice and sensorial stability during 360 days of storage of the pulp. The pulps showed no significant interaction for pH, soluble solids, acidity and color coordinated. The pH and soluble solids varied with time but remained within standards legislation. The acidity no change during the storage. The color coordinate set to the cubic model. The parameters vitamin C ranged from 190.65 to 308.45 in the pulp with preservatives, 170.95 to 299.70 in the pulp pasteurized and from 514.68 to 865.42 mg/100g in concentrated pulp, these values very expressive. Dark pigments soluble, brightness, hue*, chroma*, carotenoids, pulp content, total sugar showed significant interaction were assessed by regression with time varying storage except color coordinate b. The concentration of total sugars remained around 10.01 to 13.25% for pulps with preservatives and pasteurized,and to 24 to 27% in the concentrated pulp, which are mostly represented by sugars. The microbiological analyses confirmed the effectiveness of the processing, thermal treatment and concentration in the maintenance of the microbiological quality, once growth of microorganisms was not observed in the product during the storage period. The cashew apple nectars and juices sweetened have good acceptability in all sensory attributes. The frozen pulps cashew with preservatives, pasteurized and concentrated is viable since no significant losses occur in the quality of products.