Dans l'industrie alimentaire, les procédés de production sont souvent mis au point de manière empirique, selon des règles de bonnes pratiques. Ces méthodes présentent des lacunes, notamment au niveau de la régularité de la production. Pour modéliser et optimiser ces procédés, il est nécessaire de déterminer les propriétés physico-chimiques du produit. Nous cherchons à optimiser l'étape de tempérage du chocolat. À cette fin nous étudions la rhéologie et la cristallisation du chocolat.<p>Nous réalisons des mesures de rhéologie du chocolat suivant la méthode standard. Les résultats de ces mesures nous permettent de caractériser le comportement rhéofluidifiant de notre chocolat. Pour évaluer l'effet de différents paramètres opératoires sur la rhéologie du chocolat, nous faisons des mesures à différentes températures et pour différentes quantités de beurre de cacao. Suite à une analyse statistique des résultats, nous avons déterminé les paramètres d'une loi en puissance décrivant le<p>comportement rhéologique du chocolat. Pour approfondir la compréhension des phénomènes régissant la rhéologie du chocolat, nous avons également évalué l'influence de chaque ingrédient du chocolat sur la rhéologie du beurre de cacao. Nous montrons qu'il existe des interactions entre les particules de sucres qui sont probablement responsables du comportement rhéofluidifiant du chocolat. Nous montrons également que la présence de l'émulsifiant est indispensable pour que le chocolat puisse s'écouler.<p>La cristallisation du chocolat est analysée par calorimétrie différentielle. Nous développons un modèle de cristallisation en considérant le transfert de chaleur comme phénomène limitant. Ce modèle nous permet de déterminer les différentes formes cristallines présentes dans un échantillon de chocolat. A l'aide du modèle nous obtenons également une évaluation de la vitesse de cristallisation des différentes formes cristallines considérées. C'est un paramètre essentiel pour le dimensionnement de procédé.<p>L'étude couplée de la rhéologie et de la cristallisation nous montre que les formes cristallines les plus stables sont générées par les contraintes de cisaillement les plus élevées.<p>Enfin, dans le cadre d'applications industrielles, nous avons étudié le phénomène<p>de blanchiment du chocolat. Nous constatons que les variations de température accélèrent le phénomène de transformations polymorphiques solide-solide. Nous avons également étudié le procédé de production de la ganache. Nous avons mis en évidence que le transfert de chaleur est le phénomène déterminant de ce procédé. / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The objective of the study is to evaluate the effect of Acacia mearnsii tannin extract on balance of nutrients and efficiency of energy of steers. The experiment was conducted in a Latin Square design, with eight Holstein steers (338 ± 32,2 kg body weight (BW)). The animals have been housed in metabolism cages, fed on a diet composed by 90% corn silage and 10% concentrate at two levels of intake with or without the inclusion of Acacia mearnsii tannin extract. The treatment structure was a 2 × 2 factorial; intake, 1.2 versus 1.8 × NEm and tannin addition vs. control. The experiment was conducted in four periods of 21 days, of which the first 14 days were intended for the adaptation of the animals to the diets and the last 7 days to evaluate whole body energy balance and endogenous heat production. For measurement of heat production and nutrient balance, expired respiratory gases, urine, and feces were collected. Fecal and urine collections were taken during 7 days. Whole-body heat production (HP) was calculated by indirect calorimetry from O2 consumption and CO2 production and corrected for CH4 production and urinary N excretion using the equation proposed by Brouwer (1965). The inclusion of tannin extract had no effect on energy and nitrogen balance. The two levels of intake had effect on energy retention and whole-body heat production (P<0.001). / Este estudo foi conduzido com o objetivo de avaliar a inclusão de extrato tanífero de Acacia mearnsii a dois níveis de consumo da dieta total de bovinos sobre o balanço de nutrientes e eficiência da utilização de energia. Foram utilizados oito bovinos machos, castrados, da raça Holandês (338 ± 32,2 kg de peso corporal (PC), aleatoriamente alocados em um Quadrado Latino replicado em esquema fatorial 2 x 2 (com ou sem a inclusão de extrato tanífero x níveis de consumo). A dieta experimental foi composta de silagem de milho, milho moído e premix mineral, a relação volumoso:concentrado utilizada foi de 90:10. Foram ofertados dois níveis de consumo: 1,5 e 1,8 × Energia Líquida de mantença (Elm). O experimento foi constituído de quatro períodos de 21 dias cada, sendo 14 dias de adaptação às dietas e 7 dias de coleta de amostras. Coletas fecais e urinárias foram realizadas durante os 7 dias de coleta. A produção de calor foi calculada pela calorimetria indireta a partir do consumo de O2 e a produção de CO2 corrigido para a produção de CH4 e excreção de nitrogênio urinário utilizando equação proposta por Brouwer (1965). A inclusão do extrato tanífero não teve efeito sobre o balanço de energia e nitrogênio. Os níveis de ingestão influenciaram a retenção de energia e a produção de calor (P<0,001).

Introduction: Weight loss programs are based on inducing a negative energy balance by decreasing energy intake while increasing energy expenditure. Energy needs of obese patients are difficult to determine. The value of resting energy expenditure, as the largest component of the energy needs, is usually calculated to asses an adequate energy intake for obese patient. In clinical practice, predictive equations are most commonly used for this purpose, because of their simplicity, although many clinical studies have shown that in obese individuals they may generate errors large enough to impact the outcome of treatment. It leads to the prescription of an inadequate diet that does not meet the criterion of long-term sustainability. Objective: The aim of the thesis is to compare the values of resting energy expenditure (REE) measured by indirect calorimetry with values calculated with Harris-Benedict predictive equation in a selected group of obese individuals. Methods: The sample includes 38 subjects, 28 women and 10 men, patients of the General University Hospital in Prague. The average age is 48 ± 11,71 years, the mean BMI is 42,88 ± 9,09 kg/m2 . For each subject, resting energy expenditure was measured by indirect calorimetry and calculated by the Harris-Benedict predictive equation. Indirect...

L’oxydation des lipides est un phénomène chimique qui provoque la dégradation des qualités organoleptiques et nutritionnelles des aliments. Cette oxydation dépend de plusieurs paramètres (température, lumière, présence de métaux de transition, présence d’enzymes, état de dispersion des lipides …) qu’il est important de maîtriser notamment au cours du procédé de fabrication du produit alimentaire ou de son stockage. Dans ce contexte, l’oxydation des lipides a été étudiée, à travers la mesure des composés primaires d’oxydation, en phase continue et en émulsion eau-dans-huile. Différentes huiles alimentaires présentant des taux variés en acide α-linolénique (18:3 n-3) ont été choisies. Différentes formulations d’émulsion ont été étudiées (composition de l’interface en polyricinoléate de polyglycérol (PGPR)/monoglycérides distillés, présence de métaux pro-oxydants, d’espèces chélatantes). En revanche, la fraction volumique de phase aqueuse (40%) et le diamètre des gouttelettes d’eau (1 μm) sont maintenus constants. Parallèlement, une méthode de dosage rapide et innovante basée sur la microcalorimétrie différentielle a été mise au point pour un suivi en continu des cinétiques d’oxydation. Pour les 4 huiles végétales étudiées en phase continue et en émulsion, l’oxydabilité est liée à leur teneur en acide α-linolénique, avec la hiérarchie suivante : huile de lin > huile de caméline > huile de colza > huile d'olive. Plus la concentration en molécules pro-oxydantes (sulfate de fer) dans la phase aqueuse est élevée, plus l’oxydation des lipides est importante. L’état de valence du fer et le remplacement du fer par du cuivre n’ont pas d’impact significatif sur la cinétique d'oxydation. En revanche, il est possible de contrôler l’action pro-oxydante du fer II en jouant sur la nature du contre-ion (poids moléculaire, pouvoir chélatant) ou sur la proportion de PGPR utilisée pour stabiliser les émulsions. L’ensemble des résultats obtenus suggère que les tensioactifs lipophiles présents à l’interface eau-huile n’empêchent pas l’interaction des ions pro-oxydants avec les molécules lipidiques de la phase continue mais que leur organisation à l’interface module l’oxydation des lipides. / Oxidation is ubiquitous in lipids and causes degradation of organoleptic and nutritional qualities of foods. Lipid oxidation depends on various parameters (temperature, light, transition metals, lipid dispersion state …) that have to be controlled during food processing and storage. In this context, lipid oxidation was followed by measuring the content of primary oxidation products, for lipids in bulk phase and in water-in-oil emulsions. Different edible oils were chosen for their contents of α-linolenic acid (18: 3 n-3). Emulsions were formulated at varying polyglycerol polyricinoleate (PGPR)/distilled monoglycerides concentration ratios (surfactant ratio), with or without the presence of pro-oxydant metals or chelators. In all experiments, the aqueous volume fraction (40%) and the droplet mean diameter (1 μm) remained constant. Besides this study, an innovative and rapid method based on differential microcalorimetry was developed for monitoring the kinetics of lipid oxidation. The oxidability of the studied oils was related to their content in α-linolenic acid according the following order: linseed oil> camelina oil> rapeseed oil> olive oil. The rate of lipid oxidation increased with the iron sulfate concentration in the water phase. The iron valence or the replacement of iron by copper had no significant impact on the oxidation kinetics. However, both the chemical nature of the counter ion (molecular weight, chelating power) and the proportion of PGPR used to stabilize the emulsions were influential factors. On the whole, our results suggest that surfactants at the water-oil interface do not prevent pro-oxidant species to interact with lipids in the continuous phase but that their organization at the interface is a key parameter for controlling lipid oxidation.

Heme proteins carry out a diverse array of functions in vivo while maintaining a well-conserved 3-over-3 α-helical structure. Human hemoglobin (Hb) is well-known for its oxygen transport function. Type 1 non-symbiotic hemoglobins (nsHb1) in plants and bacterial flavohemoglobins (fHb) from a variety of bacterial species have been predicted to carry out a nitric oxide dioxygenase function. In nsHb1 and fHb this function has been linked to protection from nitrosative stress. Herein, I combine photoacoustic calorimetry (PAC), transient absorption spectroscopy (TA), and classical molecular dynamics (cMD) simulations to characterize molecular mechanism of diatomic ligand interactions with a hexa-coordinate globin from plant (rice hemoglobin), bacterial flavohemoglobins and human hemoglobin. In rice type 1 non-symbiotic hemoglobin (rHb1), the dynamics and energetics of structural changes associated with ligand photodissociation is strongly impacted by solvent and temperature, namely CO escape from the protein matrix is slower at pH = 6.0 compare to neutral pH (ns) due to the CD loop reorganization which forms a pathway for ligand escape. In human hemoglobin, exogenous allosteric effectors modulate energetics of conformational changes associated with the CO and O2 escape although the effectors impact on rate constants for ligand association is small. The conformational dynamics associated with ligand photorelease from fHbs from Cupriavidus necator (FHP) and Staphylococcus aureus (HMPSa) are strongly modulated by the presence of azole drugs indicating that drug association modulates structural properties of the heme binding pocket. In addition, we carried out a study of the formation of the DNA intercalated motif (i-motif). The formation of the structure is strongly favored at acidic pH; therefore, PAC was combined with a 2-nitrobenzaldehyde pH-jump to probe formation of the i-motif on fast timescales. i-Motif folding is two-step process with the initial protonation of cytosine residues being endothermic with ΔHfast=8.5 ± 7.0 kcal mol-1 and ΔVfast=10.4 ± 1.6 mL mol-1 and subsequent nucleation/i-motif folding (τ = 140 ns) with ΔHslow=-51.5 ± 4.8 kcal mol-1 and ΔVslow=-6.6 ± 0.9 mL mol-1. The above results indicate that PAC can be employed to study diverse biochemical reactions such as DNA folding, drug binding and ligand photorelease from proteins.

A novel UHV microcalorimeter has been used to study the interaction between calcium and three polymers: MEH-PPV, MEH-PPP and P3HT. All three polymers behave differently in their reaction kinetics with calcium. On MEH-PPV we measure 45 μJ/cm² of heat generated in excess of the heat of bulk metal growth, 120 μJ/cm² for MEH-PPP, and 100 μJ/cm² for P3HT. Comparison of the MEH-PPV and MEHPPP data indicate that the initial reaction of calcium with MEH-PPV occurs at the vinylene group. We propose, based on hypothetical models, that calcium reacts with the vinylene groups of MEH-PPV with a reaction heat of 360 kJ/mol and at a projected surface density of 1.7 sites/nm², while it reacts with the phenylene groups of MEH-PPP in a two-step process with reaction heats of 200 and 360 kJ/mol respectively, at a projected surface density of 3.5 sites/nm². Optical absorption experiments, using either a 1.85 eV diode laser or a xenon lamp coupled to a scanning monochromator, have also been performed using the same calorimeter sensor. In the case of MEH-PPV, using the laser we find an optical absorption cross-section of 3E-¹⁷ cm² per incident calcium atom at low coverages. The change in absorptance at higher coverages correlates perfectly with the population of reacted Ca atoms determined calorimetrically. The size of the absorbance cross-section, and its position just within the band gap of the polymer, are consistent with the reaction being one of polaron formation. Calcium does not appear to dope P3HT, while the photon energy range of 1.5 to 3.75 eV used in these experiments is likely too small for probing polaronic energy states in MEH-PPP. / Science, Faculty of / Chemistry, Department of / Graduate

Orientador: Claudio Airoldi / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Química / Made available in DSpace on 2018-08-26T11:26:42Z (GMT). No. of bitstreams: 1 Oliveira_CintiadosSantos_D.pdf: 3684874 bytes, checksum: 818c9e07a2f155ac52889f6ddcf9deab (MD5) Previous issue date: 2014 / Resumo: O biopolímero quitosana foi quimicamente modificado com aminas após a prévia proteção do grupo amino com benzaldeído. A reação de proteção forneceu o biopolímero BZL, que foi ativado com epicloridrina (EAC). A presença do grupo epóxido, proveniente da interação com a epicloridrina permitiu a inclusão de 2-aminometilpiridina, 2-aminopiridina, 4-aminopiridina, tetraetilenopentamina, 1,3-(aminopropilimidazol), 1-(2-aminoetil)piperazina e 1,4-bis(3-aminopropil) piperazina. Após a remoção do benzaldeído foram obtidos os biopolímeros CTN, C2MF, C4MF, TETF, IZLF, 2PPF e 3PPF, respectivamente, os quais foram caracterizados por análise elementar, difração de raios X, ressonância magnética nuclear do núcleo de carbono no estado sólido e espectroscopia na região do infravermelho. As caracterizações comprovaram o sucesso da reação de proteção dos grupos amino, bem como da remoção do benzaldeído. Os biopolímeros foram aplicados na remoção dos cátions metálicos cobre e cádmio, bem como na remoção dos corantes azul reativo 15 (RB-15), verde brilhante (BG), amarelo reativo (RY) e azul reativo (RB). Os experimentos foram realizados pelo método de batelada e os resultados obtidos foram ajustados à regressão não linear dos modelos de Langmuir, Freundlich e Sips, obtendo-se melhores ajustes ao último modelo. Os biopolímeros demonstraram uma melhor afinidade pelo cobre e dentre os corantes utilizados, uma melhor afinidade por RY. Os biopolímeros C2MF, C4MF, CTN, IZLF e TETF também foram carregados com os fármacos ibuprofenato de sódio (IBU) e diclofenaco de sódio (DCLO). Os estudos de liberação foram realizados em fluidos corpóreos simulados, obtendo-se perfis de liberação mais lentos para o DCLO. Através da calorimetria isotérmica foi investigado o processo de interação IBU ou Cu2+ com os biopolímeros. Os resultados indicaram processos endotérmicos, espontâneos e entropicamente favoráveis para o fármaco e exotérmicos, espontâneos e entalpicamente favoráveis para o cátion / Abstract: The chitosan biopolymer was chemically modified with amines after prior protection of the amino groups with benzaldehyde. The protection reaction provided the BZL biopolymer, which was activated with epichlorohydrin (EAC). The presence of epoxide groups derived from the epichlorohydrin allowed the inclusion of 2-aminomethylpyridine, 2-aminopyridine, 4-aminopyridine, tetraethylenepentamine, 1,3-(aminopropylimidazole), 1-(2-aminoethyl) piperazine and 1,4-bis(3-aminopropyl) piperazine. After bezaldehyde removal CTN, C2MF, C4MF, TETF, IZLF, 2PPF and 3PPF biopolymers were obtained, respectively, which were characterized by elemental analysis, X-ray diffraction, nuclear magnetic resonance of carbon nucleus in the solid state and infrared spectroscopy. The characterizations confirmed the success of protective reaction of amino groups as well as the benzaldehyde removal. The biopolymers were applied for the removal of copper and cadmium and also for reactive blue 15 (RB-15), brilliant green (BG), reactive yellow (RY) and reactive blue (RB) dyes. The experiments were carried out by batch method and the results were fitted with non-linear regression of the models of Langmuir, Freundlich and Sips, where the better fit was obtained using the last model. The biopolymers demonstrated better affinity for copper and among the dyes used, the best affinity was observed for RY. The C2MF, C4MF, CTN, TETF and IZLF biopolymers were also loaded with sodium ibuprofen (IBU) and diclofenac (DCLO) drugs. The release investigations were performed in simulated body fluids, resulting in slower release profile for DCLO. Through isothermal calorimetry processes, the interaction of IBU or Cu2+ with biopolymers was studied. The results indicated endothermic, spontaneous and entropically favorable processes for the drug and exothermic, spontaneous and favorable enthalpy process for the cation / Doutorado / Quimica Inorganica / Doutora em Ciências

Orientador: Jose de Alencar Simoni / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica / Made available in DSpace on 2018-08-14T14:10:59Z (GMT). No. of bitstreams: 1 Curti_GabrielJeronymo_M.pdf: 9486555 bytes, checksum: d62a8756cd8f980fa037df03ee42b8ab (MD5) Previous issue date: 2009 / Resumo: Esse estudo investiga a influência de práticas agrícolas na atividade microbiana de solos, utilizando-se a calorimetria. Quatro amostras de solo foram coletadas no município de Pradópolis, São Paulo, Brasil (21°19'8'' S 48°7'16' ' W), onde se praticavam dois diferentes tipos de manejo: solo sujeito à queima periódica, e solos não sujeitos à queima, em que, 2, 4, e 7 cortes consecutivos da cultura de cana foram observados. Nesses solos também houve contínuo incremento de cobertura vegetal. O estudo calorimétrico corresponde ao registro da energia dissipada em função do tempo, utilizando-se glicose como substrato. As amostras foram também caracterizadas por diversas análises químicas (teor de carbono total e acidez), físicas (porosidade, densidade, argila dispersa), biológica (número de microorganismos), e por técnicas de análise térmica como TGA, e DSC. Os resultados de calorimetria evidenciam diferenças entre os diferentes manejos em relação a parâmetros como: eficiência de assimilação da matéria orgânica (hH), constante de crescimento microbiano (k), e a quantidade biomassa viva formada (DX). O solo associado a práticas de queimada apresentou uma baixa eficiência percentual de assimilação de matéria orgânica (hH = 53 %), um valor só comparável ao solo com 4 cortes. Também foi o solo que apresentou a menor constante de crescimento (k = 2,09 x 10 min) e um dos maiores valores de peak time (598 minutos). Embora o crescimento microbiano tenha sido mais lento para o solo com queima, o valor de energia anabolizada ficou em torno de 50 %. Por outro lado, a anabolização como matéria orgânica viva (DX) foi a mais baixa de todas (181 mg ou 34% de hH), enquanto que para os outros solos DX foi praticamente igual a hH. / Abstract: This study investigates the influence of tilling practices on the soil microbial activity, through the use of calorimetric techniques. Four soil samples were collected at the municipality of Pradópolis, São Paulo, Brazil (21°1 9'8''S 48°7'16''W), where two kinds of different agricultural managements were used: a soil subjected to periodical burning, and soils do not subject to burning, where subsequent 2, 4, and 7 cuts of the sugarcane plantation were done, with continuous increase of the vegetal covering. The calorimetric study corresponds to follow the heat flow versus time curves, for a mass of glucose amended to the soil. The sample soils were characterized through chemical analysis (total carbon and acidity), physical analysis (porosity, density, disperse clay), biological analysis (microorganism numbers) and more specifically by TGA, DSC and microcalorimetry. The calorimetric results show differences depending on the tilling practice, respect to some parameters evaluated: efficiency of organic material assimilation (hH), specific microbial growth constant (k), and the amount of live biomass formed (DX). The soil where the burning is used showed a low percentual efficiency of organic material (hH = 53 %), a value close to the soil with 4 cuts. It was verified to the burning condition the smallest value of growing rate (k = 2.09 x 10 min) and a relatively great value of peak time (598 minutes) for this sample. For the burning soil the microbial growth constant was the lowest one but the percentual of assimilated energy stayed close to 50% to this sample. Similarly, the live organic material anabolism (DX) was the lowest value registered (181 mg ou 34% of hH ), while this parameter was practically equal to hH for the other soil samples. / Mestrado / Físico-Química / Mestre em Química

Submitted by Haroudo Xavier Filho (haroudo.xavierfo@ufpe.br) on 2016-04-14T17:04:05Z No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) Dissertação_Taynara_Lins.pdf: 2092995 bytes, checksum: 279f65308ce3391337c22f33dbbe9243 (MD5) / Made available in DSpace on 2016-04-14T17:04:05Z (GMT). No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) Dissertação_Taynara_Lins.pdf: 2092995 bytes, checksum: 279f65308ce3391337c22f33dbbe9243 (MD5) Previous issue date: 2015-02-25 / CNPq / Este estudo teve como finalidade desenvolver metodologias analíticas para os estudos de caracterização do estado sólido do fármaco atorvastatina cálcica e, também, das suas dispersões sólidas pelas correlação das técnicas difratometria de Raios X (DRX), espectroscopia de infravermelho (FTIR) e analise térmica (DSC e TG). A atorvastatina cálcica (ATC) é um agente redutor de lipídios sintético, que já tem muitos polimorfos relatados na literatura. No estudo de caracterização no estado sólido do fármaco, foram obtidos cristais da ATC com solventes de graus de polaridade diferentes e foi observado que os solventes clorofórmio, etanol e metanol levaram a formação de uma estrutura cristalina mais amorfa, e essa alteração estrutural foi perceptível no FTIR com alteração na banda do estiramento da hidroxila e pelos dados de DSC como diminuição da entalpia e desaparecimento do pico de fusão. Enquanto que, solventes éter e acetato de etila não levaram a mudança no habito cristalino quando comparado com o fármaco antes do processo de recristalização. As dispersões sólidas foram feitas com 5 surfactantes diferentes (carbopol®, hidroxipropil metil celulose (HPMC), lauril sulfato sódio, polietileno glicol (PEG) 6000 e carbopol-ultrez® 20) e pela correlação do dados DRX, FTIR e DSC foi visto que a dispersão com carbopol-utlrez foi a que apresentou grande interação com mudanças nas banda de absorção e desaparecimento do pico de fusão. Ao avaliarmos a estabilidade das dispersões por termogravimetria, observou-se que todas elas tinham menor estabilidade que a ATC. Esses resultados apontam para a utilidade de técnicas de análise térmica como uma ferramenta de triagem relevante para a caracterização do estado sólido durante o desenvolvimento de formulação. Através da análise multivariada foi possível estabelecer a correlação entre a técnicas estudadas mostrando a relevância da utilização destas na avaliação dos parâmetros de controle qualidade de processos e produtos farmacêuticos. / This study aimed to develop analytical methods for the characterization studies of solid state drug atorvastatin calcium and also their solid dispersions by the correlation of techniques: X-ray diffraction (XRD), infrared spectroscopy (FTIR) and thermal analysis (DSC and TG). The atorvastatin calcium (ATC) is a reducing agent synthetic lipids, which already has many polymorphs reported in the literature. In the characterization studies in the solid state of the drug, ATC crystals were obtained with different degrees of polarity solvent and it was observed that the solvents chloroform, ethanol and methanol led to formation of a more amorphous crystal structure, and this structural change was noticeable in FTIR with changes in the band of the hydroxyl stretch and by the DSC data as decreased enthalpy and disappearance of the melting peak. While, ether and ethyl acetate solvents did not lead to change in the crystal habit when compared with the drug before the recrystallization process. Solid dispersions were made with 5 different surfactants (Carbopol®, hydroxypropyl methyl cellulose (HPMC), sodium lauryl sulfate, polyethylene glycol (PEG) 6000 and carbopol-ultrez® 20) and by the correlation data of XRD, FTIR and DSC was seen that the dispersion with carbopol-utlrez showed the great interaction with changes in absorption band and disappearance of the melting peak. In evaluating the stability of the dispersions by thermogravimetric analysis, it was observed that all of them had lower stability than ATC. These results point to the utility of thermal analysis techniques as an important screening tool for the characterization of the solid state during the development of formulation. Through multivariate analysis was possible to establish the correlation between the techniques studied shows the importance of using these in the evaluation of the quality control parameters of process and pharmaceuticals.

Submitted by Haroudo Xavier Filho (haroudo.xavierfo@ufpe.br) on 2016-04-14T18:12:12Z No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) Dissertação_Waleska Vianna.pdf: 2762250 bytes, checksum: 49ac43d4d17ee59b86aa1081a15fb0ff (MD5) / Made available in DSpace on 2016-04-14T18:12:12Z (GMT). No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) Dissertação_Waleska Vianna.pdf: 2762250 bytes, checksum: 49ac43d4d17ee59b86aa1081a15fb0ff (MD5) Previous issue date: 2015-02-25 / CAPES / O besilato de anlodipino é um antagonista dos canais de cálcio, utilizado como um anti-hipertensivo e anti-isquêmico, sendo utilizado como uma mistura racêmica dos enantiômeros S e R, dos quais o S-anlodipino é o que apresenta maior atividade como bloqueador de cálcio. Por tanto, o objetivo desse estudo foi caracterizar as formas cristalinas do besilato de anlodipino e correlacionar os parâmetros térmicos e analíticos das dispersões sólidas do besilato de anlodipino obtidas por liofilização. Os ângulos vistos no DRX demonstraram a presença de uma estrutura cristalina anidra, para o AMB. Os deslocamentos nos comprimentos de onda no espectro de infravermelho (FTIR) do cristal do AMBACt corroboraram com os resultados do DRX que apresentou mudança no tamanho dos cristalitos, além disso a curva de DSC apresentou dois picos endotérmicos diferentemente do fármaco, com apenas um processo endotérmico e grau de pureza de 96%. A energia cinética de ativação (Ea = 121,6 KJ mol-1 ±1,2), o fator de frequência (A = 27,87 ± 4,1 min-1), e a ordem de reação (n = 0) da etapa principal da decomposição térmica do AMB foram realizadas de acordo com o Modelo de Ozawa. No estudo das dispersões sólidas, os dados do DRX para o AMBHPMC apresentou amorfização e essa alteração no arranjo cristalino também foi evidenciada nos resultados encontrados no FTIR, com deslocamentos nas bandas de intensidade, supressão e aparecimento de novas bandas. Além disso, o método termoanalítico mostrou supressão e deslocamento dos picos de fusões das dispersões sólidas, e perda de massa diferente do fármaco. Portanto, juntas, as técnicas colaboraram para a caracterização das formas cristalinas, e nos estudos de compatibilidade fármaco-excipiente através avaliação das interações físico-químicas nas dispersões sólidas. / The amlodipine besylate is a calcium channel antagonist used as antihypertensive and anti- ischemic , and used as a racemic mixture of R and S enantiomers , of which the S- amlodipine is what is more active as blockers calcium. Therefore, the aim of this study was to characterize the crystalline forms of amlodipine besylate and correlate the thermal and analytical parameters of solid dispersions of amlodipine besylate obtained by lyophilization. The angles viewed XRD showed the presence of an anhydrous crystalline structure for the AMB. The shifts in wavelengths in the infrared spectrum (FTIR) of the AMBACt crystal corroborate with the results of the XRD which showed change in the size of the crystallites, furthermore the DSC curve showed two endothermic peaks unlike the drug with only one process endothermic and purity of 96%. The activation kinetic energy (Ea = 121.6 kJ mol-1 ± 1.2), the frequency factor (A = 27.87 ± 4.1 min-1) and the reaction order (n = 0) of the main stage of AMB thermal decomposition were performed according to the Ozawa model. In the study of of the solid dispersions, the XRD data for AMBHPMC which showed amorphization and this change in the crystalline arrangement was also evidenced in the results found in the FTIR, with shifts in intensity bands, suppression and appearance of new bands. Also, the thermal method proved suppression and displacement of the melting peaks of the solid dispersions and loss of mass different than drug. Porting together the characterization techniques contributed to the evaluation of crystalline forms, and of the physicochemical interactions in solid dispersions.