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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
11

Investigation of the Chemical Protection Capacity of Common Shoe Materials in Undergraduate Laboratories

Lawson, Sarah E 01 May 2015 (has links)
The objective of this study was to evaluate the chemical resistance of common shoe materials regularly worn in undergraduate chemistry laboratories by subjecting the materials to hydrochloric acid and sodium hydroxide. The materials tested were leather, canvas cotton, and polyester. Due to the lack of restriction on undergraduate laboratory footwear, the research discussed in this thesis is important to undergraduate universities. Currently, many universities across the nation only require undergraduate students to wear close-toed, close-heeled shoes in chemistry laboratories, and often the resistance of the shoe material to acids and bases may not be taken into careful consideration. Overall, the results of this experiment revealed that exposure to the different chemical concentrations of NaOH and HCl did not appear to negatively affect the structural integrity of the fabrics, but according to the mass spectrometry results gathered in this experiment, the three fabrics differed in individual complexities as well as in the compounds extracted following acid and base treatments.
12

Formulation, caractérisation et mise en œuvre des barrières perméables réactives à base de phosphate de calcium, utilisation pour la fixation de polluants / Formulation, caracterization and implementation of permeable reactive barriers based on calcium phosphate

Raii, Mohamed 12 December 2012 (has links)
L'objectif principal de cette thèse est la formulation des mélanges stables contenant l'hydroxyapatite gel synthétisée (Ca-HAGel). Le comportement rhéologique des mélanges Eau/(sulfate de calcium) et hydroxyapatite/(sulfate de calcium) a été étudié. Les résultats ont montré que tout les mélanges sont caractérisés par un comportement rhéologique rhefluidifiant et thixotrope. Le potentiel zeta a été utilisé dans cette étude pour mieux appréhender les interactions entre les particules et leur effet sur le comportement des mélanges. La fixation de sulfate sur la surface de Ca- HA favorise la stabilité de la structure du Ca-HAGel. Les analyses de caractérisation effectuées sur les formulations ont montré la formation de nouveaux composés tels que le sulfate-phosphate de calcium hydrate et l'Ardealite. Les tests de lixiviation et de percolation ont révélé que le taux de relargage de soufre et strontium à partir des sous-produits de gypse était négligeable pour les mélanges contenant Ca-HAGel. Ca- HAGel stabilise les métaux lourds relargués à partir du gypse et plâtre. Les particules du gypse améliorent les performances hydrauliques de Ca-HAGel et le plâtre hydraté stabilise la structure de Ca-HAGel par la formation des particules agglomérées. Le test colonne effectué sur la formulation AWPG2 a montré une grande performance à retenir le plomb et le cadmium avec des capacités de rétention de plus de 99% et 88% respectivement. Le traitement des métaux lourds était lié aux particules de Ca-HA et aux phosphate et calcium libres. La formulation AWPG2 peut être utilisée dans les barrières perméables réactives pour traiter les eaux souterraines contaminées. / The main purpose of this thesis was the formulation of stable blends based on synthesized hydroxyapatite-gel (Ca-HAGel). The rheological behavior of water−calcium sulfates and hydroxyapatite−calcium sulfates blends was considered in this study. The results show that all blends and formulations exhibit a shearthinning effect and thixotropic behavior. The ζ potential was used in this study to understand the interaction between particles and its effect on the global behavior of the blends. Fixation of sulfate on Ca-HA surface promotes the stability of Ca-HAGel suspension. Characterization analysis of formulation shown the presence of new compounds such as calcium sulfate-phosphate hydrate and Ardealite. Leaching and percolation tests revealed that the release rate of sulfur and strontium from gypsum by-product was negligible in blends based on Ca- Agel. Ca-HAGel was stabilized the heavy metals released from plaster and gypsum. Gypsum particles enhanced hydraulic performances of Ca-HAGel and hydrated plaster stabilized Ca-HAGel structure by the formation of agglomerated particles. Column test carried out on AWPG2 blend revealed high removal performances for lead and cadmium with retention capacity of 99% and 88% respectively. The reactivity was related to Ca-HA and free calcium and phosphate contained in the selected formulation. AWPG2 blend is to be used as permeable reactive barrier for in-situ contaminated groundwater remediation
13

Vitamin Stability and Water-Solid Interactions

Adrienne Lea Voelker (9510965) 16 December 2020 (has links)
<p>This dissertation investigates two major structure-function relationships important to food science: vitamin stability and water-solid interactions. Thiamine, vitamin B<sub>1</sub>, is an essential micronutrient in the human diet. While thiamine is found naturally and as a fortification supplement in many foods, it is chemically unstable on exposure to heat and some co-formulated ingredients, with degradation exacerbated in prolonged shelf-life products. The instability of thiamine is a concern for the development of dietary deficiencies, which are prevalent even in developed countries; however, thiamine stability is not widely studied in the food or pharmaceutical industries. Thiamine is commercially available in two salt forms: thiamine mononitrate (TMN) and thiamine chloride hydrochloride (TClHCl). This study focused on documenting the storage stability of thiamine in solution, considering the effects of which commercially available salt form of the vitamin was used, vitamin concentration, pH, and ions present in solution by monitoring chemical stability and degradation kinetics over a 6-month to 1-year period following storage at 25-80ºC, and expanded these studies into food systems (bread doughs). The results from these studies, including the reaction kinetics of thiamine degradation, the degradation pathway, and the sensory impacts of the degradation products formed, especially as affected by pH and food matrix, can be used to improve thiamine stability and delivery in foods.</p><p></p><p>The studies of water-solid interactions in this dissertation covered two topics: 1) the effects of formulating a variety of food-relevant additives on the crystallization tendency of amorphous sucrose; and 2) the effects of formulation on the moisture sorption behaviors and physical stability of spices, herbs, and seasoning blends. Sucrose lyophiles were co-formulated with a variety of additives and stored at 11-40% relative humidity (RH). The structural compatibility of sucrose with the additive, and related intermolecular interactions, dictated the tendency of the additive to either delay, prevent, or accelerate sucrose crystallization. Spices, herbs, and seasoning blends were exposed to increasing RH (23-75%) and temperature (20-50ºC) to determine the effect of storage and formulation on a variety of physical properties. In general, as complexity of blends increased, physical stability decreased. While this dissertation covers a wide variety of food chemistry and food materials science topics, including vitamin chemical stability, amorphous sucrose physical stability, and moisture sorption behaviors of spices, herbs, and seasoning blends, the findings provide valuable information on the chemical and physical stability of ingredient systems and how the structure-function relationships of the systems can be controlled for optimal ingredient functionality.</p><p></p>
14

Structural studies of organic crystals of pharmaceutical relevance : correlation of crystal structure analysis with recognised non-bonded structural motifs in the organic solid state

Essandoh, Ernest January 2009 (has links)
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.
15

Estudos da lipofilia e estabilidade química de inibidores de cisteíno proteases / Lipophilicity and chemical stability of inhibitors of cysteine proteases

Silva, Samelyn da Costa Martins 14 June 2018 (has links)
O estudo das propriedades físico-químicas é essencial na fase de otimização e desenvolvimento de substâncias bioativas. A lipofilia e a estabilidade química de candidatos a fármacos são extremamente importantes e devem ser determinadas nas fases iniciais da descoberta de fármacos. A determinação da lipofilia dos compostos bioativos foi feita utilizando Membrana Artificial Imobilizada (IAM) para obtenção do logKw. Já a bioanálise qualitativa da estabilidade química de algumas substâncias em meio de cultura foi estudada utilizando um sistema RP-HPLC-MS com fonte de ionização eletrospray e analisador ion trap. Estruturas químicas de dipeptidil nitrilas foram sintetizadas pelo grupo tendo como alvo a inibição de cisteíno proteases a fim de combater a Doença de Chagas e alguns tipos de carcinomas. O trabalho foi realizado a fim de expandir as análises para uma série de derivados do NEQ0409 de forma que foi estabelecido um mapa com aumento da lipofilia de acordo com as modificações estruturais nas substâncias. Desta maneira foi possível obter uma relação estrutura-propriedade (SPR), além da análise do perfil de degradação e/ou estabilidade de algumas das substâncias de interesse, demonstrando que as substâncias analisadas apresentam potencial para continuarem na fase de desenvolvimento. / The study of physicochemical properties is essential in the optimization and development phases of bioactive substances. The lipophilicity and chemical stability of drug candidates are extremely important and should be determined in the initial steps of the drug discovery program. Therefore, the determination of the lipophilicity of the bioactive compounds was done using immobilized artificial membrane (IAM) to obtain logKw. Furthermore, the qualitative bioanalysis of the chemical stability of some substances in culture medium was studied using a RP-HPLC-MS system with electrotropray ionization source and ion trap analyzer. A series of dipeptidyl nitriles was synthesized by the group aiming to inhibit cysteine proteases as an alternative therapeutic approach for Chagas disease and some types of carcinomas. The work was carried out to expand the analyses for a series of derivatives of NEQ0409, so that a map of dipeptidyl nitriles with higher lipophilic characteristics was established according to the substituents of the new compounds. In this way, it was possible to obtain a structure-property relationship (SPR), besides the analysis of the degradation and/or stability profile of some of the substances of interest. All-in-all, these results suggest that dipeptidyl nitrile derivatives are potential candidates for further development.
16

Development of Safe-by-Design Nano-composites for Food Packaging Application / Conception raisonnée de nanomatériaux sûrs pour l'homme et l'environnement

Nasiri, Aida 23 February 2017 (has links)
Ce projet contribue à développer la prochaine génération de nano-emballages en utilisant une approche plus sûre et éco-conçue avec des avantages directs à la fois pour l'environnement et la sécurité des consommateurs. Les emballages alimentaires constituent l’un des principaux secteurs d’applications des nanotechnologies avec des enjeux environnementaux prometteurs de substitution des pétro-plastiques par des bio-plastiques et de réduction des pertes et gaspillages alimentaires grâce à des emballages plus performants, de type actifs et intelligents. Dans le cas de matériaux nano-composites (matrice polymérique contenant des nano-particules) destinés au contact alimentaire, le risque majeur en terme de santé humaine est lié à leur impact sur la migration de composés indésirables de l’emballage vers l’aliment (stabilisants UV, antioxydants, plastifiants, etc) qui peuvent avoir des effets néfastes en fonction des doses et durées d’exposition. Ces interactions contenant/contenu sont soumises à une réglementation européenne dont l’objectif est la protection de la santé du consommateur en fixant des limites de migration spécifique pour tous les composés supposés entrer dans la composition des matériaux plastiques dédiés au contact alimentaire. Dans le cas des nanomatériaux, la présence de nanoparticules est susceptible de modifier les interactions entre le polymère et les additifs et par voie de conséquence leurs propriétés de transfert. Ainsi, la formalisation des phénomènes de migration de l’emballage vers l’aliment établie sur des matériaux plastiques ne contenant pas de nanoparticules ne peut pas être directement transposée au nano-matériaux. De plus la présence de ces nanoparticules peut profondément modifier l’éco-toxicité environnementale du système matrice- nanoparticule -additif.La présente étude vise à comprendre et contrôler l’impact des structures nanocomposites (matrice polymérique contenant des nano-particules) sur les propriétés de transport (diffusivité et solubilité) des nanoparticules et des additifs chimiques en condition d’usage. À cet égard, il est nécessaire de combler le déficit de connaissances dans a caractérisation de la structure 3D, des propriétés physico-chimique et des interactions aux interfaces entre nanoparticules et matrice dans les nanomatériaux. Devant la complexité du système étudié, la modélisation est indispensable pour représenter (simplifier sans pour autant perdre trop de connaissances) la structure 3D des nanomatériaux et simuler, reproduire puis prédire, l’évolution de leurs propriétés de transfert en fonction des paramètres structurels et en condition d’usage. La modélisation des transferts est également indispensable pour, dans une approche d’ingénierie inverse, éco-concevoir et dimensionner à façon des nano-emballages sûrs pour l’Homme et l’Environnement. Dans cette optique une démarche de modélisation multi-échelle des relations structure/propriétés de transfert de masse a été mise en place sur des matériaux nanocomposites ciblés choisis pour leur pertinence dans le domaine de l’emballage alimentaire. / The market of nanotechnologies is dominated by the food packaging area which amounts more than 20% of the total nanotechnologies market in 2015. However, the wide-scale use of nanomaterials raises important questions about environmental and safety issues that could hinder their development. In the case of plastics intended to be in contact with food, the risk of contamination concerns not only the nanoparticles but also all the chemical additives added during the material processing. The presence of nanoparticles is susceptible to modify the interactions between polymer and the additives with a possible change in their transport properties and therefore the food contamination.The present work aims at identifying the relationship between the structural characteristic and the transport properties (diffusivity and solubility) of nanoparticles and chemical additives incorporated in nanocomposites. In this regard, it is necessary to fill the gap of knowledge in 3D nanostructure characterization and a multi-scale modeling of mass transfer properties of nanocomposites in real usage conditions.In this way, polyethylene and nanoclay were selected based on the best compromise between real potential applications and the scientific knowledge previously published and eventually the nanocomposites were synthesized with LLDPE, Cloisite20 and a compatibilizer by melt intercalation method.The nanocomposite structure was characterized using TEM, X-ray nanotomography, TGA and XRD then submitted to migration tests undertaken in contact with different food simulants which represent various types of food (aqueous, acid, alcoholic) following the recommendation of the European regulation on the food contact material. To evaluate the positive or adverse effects of the nanomaterials on the contamination of the food by chemical additives which are usually incorporated with the plastic packaging, the virgin polymer and nanocomposite material were spiked with a mixture of the additives exhibiting various volatility, polarity and molecular weight. Then, the transport properties (i.e inertia) of nanocomposite structure was distinctively investigated on kinetic (apparent diffusion coefficient) and thermodynamic (partition coefficient) considerations.The results indicated that nanoclay addition in plastic materials favorably reduced the migration of additives by modifying both their diffusivity in the polymer and their partition between the polymer and the food simulant. However, while the partition coefficient of additives increases in nanocomposite in comparison to pure LLDPE for the samples in contact with all types of food simulants, the reduction of diffusion coefficient is significantly dependent on the nature of the food simulant in contact. Hence, it can be concluded that the major role in the migration of additives is not played by the imposed tortuosity path, but by the factors such as the affinity between the base polymer and simulants as well as the effects of simulants on swelling and crystallinity of the samples. Moreover, the effect of additive-related parameters and the structural parameters were assessed and put in perspective with their impact on the transport properties of nanostructures. Integrating the results of characterization and transfer properties led to an improved understanding of the influence of structure of nanocomposites on their mass transfer properties and therefore on the suitability of using them as food contact materials.
17

Estudos da lipofilia e estabilidade química de inibidores de cisteíno proteases / Lipophilicity and chemical stability of inhibitors of cysteine proteases

Samelyn da Costa Martins Silva 14 June 2018 (has links)
O estudo das propriedades físico-químicas é essencial na fase de otimização e desenvolvimento de substâncias bioativas. A lipofilia e a estabilidade química de candidatos a fármacos são extremamente importantes e devem ser determinadas nas fases iniciais da descoberta de fármacos. A determinação da lipofilia dos compostos bioativos foi feita utilizando Membrana Artificial Imobilizada (IAM) para obtenção do logKw. Já a bioanálise qualitativa da estabilidade química de algumas substâncias em meio de cultura foi estudada utilizando um sistema RP-HPLC-MS com fonte de ionização eletrospray e analisador ion trap. Estruturas químicas de dipeptidil nitrilas foram sintetizadas pelo grupo tendo como alvo a inibição de cisteíno proteases a fim de combater a Doença de Chagas e alguns tipos de carcinomas. O trabalho foi realizado a fim de expandir as análises para uma série de derivados do NEQ0409 de forma que foi estabelecido um mapa com aumento da lipofilia de acordo com as modificações estruturais nas substâncias. Desta maneira foi possível obter uma relação estrutura-propriedade (SPR), além da análise do perfil de degradação e/ou estabilidade de algumas das substâncias de interesse, demonstrando que as substâncias analisadas apresentam potencial para continuarem na fase de desenvolvimento. / The study of physicochemical properties is essential in the optimization and development phases of bioactive substances. The lipophilicity and chemical stability of drug candidates are extremely important and should be determined in the initial steps of the drug discovery program. Therefore, the determination of the lipophilicity of the bioactive compounds was done using immobilized artificial membrane (IAM) to obtain logKw. Furthermore, the qualitative bioanalysis of the chemical stability of some substances in culture medium was studied using a RP-HPLC-MS system with electrotropray ionization source and ion trap analyzer. A series of dipeptidyl nitriles was synthesized by the group aiming to inhibit cysteine proteases as an alternative therapeutic approach for Chagas disease and some types of carcinomas. The work was carried out to expand the analyses for a series of derivatives of NEQ0409, so that a map of dipeptidyl nitriles with higher lipophilic characteristics was established according to the substituents of the new compounds. In this way, it was possible to obtain a structure-property relationship (SPR), besides the analysis of the degradation and/or stability profile of some of the substances of interest. All-in-all, these results suggest that dipeptidyl nitrile derivatives are potential candidates for further development.
18

Otimização de obtenção de um extrato aquoso de milho roxo (Zea mays L.) rico em antocianinas e perfil de degradação / Optimization of obtaining an aqueous extract of purple corn (Zea mays L.) rich in anthocyanins and degradation profile.

Stanquevis, Regina 23 October 2013 (has links)
O milho roxo (Zea mays L.), cultura tradicional da região Andina, é conhecido por apresentar alto conteúdo de antocianinas. As antocianinas apresentam diversas propriedades biológicas demonstradas em estudos in vitro e in vivo; entre elas, alto poder antioxidante, atividade anti-inflamatória e quimiopreventiva; entretanto são compostos que se degradam facilmente. Assim, o objetivo deste trabalho foi obter um extrato aquoso rico em antocianinas, a partir do milho roxo, e estudar a estabilidade química das antocianinas presentes frente ao pH e temperatura. Inicialmente o milho roxo comercial, utilizado como matéria prima, foi caracterizado por CLAE-DAD-ESI-MS/MS por apresentar cinco derivados de cianidina, três derivados de peonidina, três derivados de pelargonidina, dois derivados de quercetina e dois derivados de isoramnetina, com presença de acilação nas antocianinas. O teor de antocianinas totais foi de 4,61 mg/g, sendo 3,16 mg cianidina 3-glucosídeo eq./g, 0,63 mg pelargonidina/g e 0,81 mg peonidina/g, além de 1,19 mg quercetina/g e 1,06 mg ácido protocatecúico/g. Para a otimização da obtenção do extrato aquoso e estudo de degradação térmica das antocianinas, foi realizado o delineamento experimental para análise de superfície de resposta. Um delineamento fatorial 33 (15 ensaios com 3 repetições do ponto central) foi aplicado para avaliar o efeito de três fatores,em três níveis, para a obtenção do extrato aquoso. Os fatores incluídos foram temperatura (70ºC, 95ºC e 120ºC), tempo de extração (10, 50 e 90 min) e pH da solução (3,0, 5,0 e 7,0). Foram avaliadas três respostas: teor de antocianinas monoméricas, teor de ácido protocatecúico e capacidade antioxidante, os quais foram encontrados: (a) para antocianinas monoméricas, a melhor condição de extração foi obtida no menor valor de pH (3,0) e tempo (10 min), com temperatura intermediária (95ºC); (b) para o ácido protocatecúico, a melhor concentração foi obtida em condições de maior valor de pH (7,0) e tempo (90 min), ou seja, oposto à condição anterior, com temperatura intermediária (95ºC); (c) para a capacidade antioxidante, a melhor condição foi obtida quando preparou-se o extrato no ponto central dos níveis (pH 5,0), tempo 50 min e temperatura (95ºC). Os modelos referentes às respostas de teor antocianinas monoméricas e teor de ácido protocatecúico foram validados, apresentando valores 40,30 mg cianidina 3-glucosídeo eq./L e 0,57 mg/100 mL, respectivamente. Os flavonoides identificados no extrato aquoso de milho roxo foram semelhantes à composição do milho roxo comercial, entretanto, com considerável degradação de derivados de cianidina e peonidina, principalmente aciladas, a ácido protocatecúico e ácido vanílico, respectivamente. Assim, os resultados sugerem que um extrato aquoso de milho roxo rico em antocianinas é obtido em condições de extração de menor valor de pH, onde as antocianinas estão em sua forma mais estável. Porém, quando esse extrato aquoso é exposto a maiores valores de pH e/ou alta temperatura, pode ocorrer degradação das antocianinas presentes aos seus respectivos ácidos fenólicos. / Purple corn (Zea mays L.), traditional culture of the Andean region, is known for its high content of anthocyanins. Anthocyanins exhibit several biological properties demonstrated in in vitro and in vivo, among them, high antioxidant, anti-inflammatory and chemopreventive activities, however they are unstable. The objective of this study was to obtain an aqueous extract rich in anthocyanins from purple corn and study the chemical stability of anthocyanins. Initially commercial purple corn, used as raw material, was characterized by HPLC-DAD-ESI-MS/MS by presenting five cyanidin derivatives, three peonidin derivatives, three pelargonidin derivatives, two quercetin derivatives and two isorhamnetin derivatives, with acylation in some anthocyanins. The anthocyanin content was 4.61 mg/g, which 3.16 mg cyanidin 3-glucoside eq./g, 0.63 mg pelargonidin/g and 0.81 mg peonidin/g, in addition 1.19 mg quercetin/g and 1.06 mg protocatechuic acid/g. To optimize the aqueous extract and study thermal degradation of anthocyanins, an experimental design was performed for response surface analysis. A 33 factorial design (15 trials with 3 replicates of the center point) was applied to evaluate the effect of three factors at three levels, to obtain the aqueous extract. The factors included were temperature (70°C, 95°C and 120°C), extraction times (10, 50 and 90 min) and pH solution (3.0, 5.0 and 7.0). Three variables were evaluated: monomeric anthocyanin content, protocatechuic acid content and antioxidant capacity, which were found: (a) for monomeric anthocyanins content, the best extraction condition was obtained at lower pH (3.0) and time (10 min), and intermediate temperature (95°C); (b) for protocatechuic acid content, the optimal concentration was obtained under higher pH (7.0) and time (90 min), opposite to the previous condition, with intermediate temperature (95°C); (c) for antioxidante capacity, the best condition was obtained when the extract was prepared at the midpoint of levels pH 5.0, time 50 min and 95°C. The mathematicals models concerting monomeric anthocyanins content and protocatechuic acid content has been validated, with values of 40.30 mg cyanidin 3-glucoside eq./L and 0.57 mg/100 mL, respectively. The flavonoids profile in the aqueous extract of purple corn were similar to the composition of commercial purple corn, however, with considerable degradation of cyanidin and peonidin derivatives, mainly acylated form, to protocatechuic acid and vanillic acid, respectively. Therefore, the results suggests that an aqueous extract of purple corn rich in anthocyanins can be obtained at lower pH, where the anthocyanins are in their most stable form. However, when the aqueous extract is exposed to higher pH and/or high temperature, anthocyanins degradation may occur to their respective phenolic acids.
19

The role of pharmaceutical excipients in the solid-state degradation of Gabapentin

Tinmanee, Radaduen 01 July 2015 (has links)
Drug instability in solid dosage forms includes chemical or physical processes involving covalent or polymorphic transformations wherein different polymorphs possess crystal structure differences. Gabapentin chemically degrades by intramolecular cyclization to gabapentin-lactam (lactam) in the solid-state. Additionally, gabapentin undergoes polymorphic solid-state transformations. A kinetic model was developed to describe the environmental and excipient effects on chemical and physical instability associated with milling induced stress and subsequent storage under controlled temperature and humidity conditions. Reaction mixtures were generated by co-milling gabapentin Form II with various excipients. The effects of environmental conditions were studied by storing reaction mixtures at 40-60 ºC and 5-50 %RH. The chemical and polymorphic compositions of the reaction mixtures were measured as a function of time using a combination of chromatographic method, 13C ssNMR and XRPD. Degradation models that describe the relationship between polymorphs and degradation product in a series of sequential or parallel steps were devised based on analysis of the resultant concentration time profiles. Model parameters were estimated using non-linear regression and Bayesian methods and evaluated in terms of their quantitative relationship to compositional and conditional variations. In reaction mixtures composed of co-milled gabapentin and excipients, gabapentin was found to exist in three forms: anhydrous polymorph II and III and gabapentin-lactam. A fourth form (II*) was observed based on initial degradation kinetics and was hypothesized to be a crystal-disordered form generated by mechanical stress. The effect of environment moisture was to decrease the net rate of lactam formation by facilitating polymorphic transformation kinetics and crystal annealing. However, excipient blocked the catalytic moisture effect on polymorphic transformations. The key features of our model are first-order physical state transitions of II* and III to II, first-order degradation of II* to lactam and autocatalytic lactamization of II and III. For chemical transitions, no humidity effect was present but the catalytic effects of excipients on the conversion of II and III → lactam were observed. For physical transitions, excipient primarily influenced the physical state transitions of II*and III → II through its ability to interact with humidity and the degree of contact between excipient and substrate.
20

Estudo do crescimento, estabilidade física, química e termogravimétrica com rações para camarão marinho Litopenaues vannamei

Capistrano Sobrinho, David 30 May 2011 (has links)
Made available in DSpace on 2015-04-17T14:49:14Z (GMT). No. of bitstreams: 1 arquivototal.pdf: 1474589 bytes, checksum: b9383bfcffc47669804f85a9cf07dd34 (MD5) Previous issue date: 2011-05-30 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / The Aquaculture has been a fast developed in recent years and the shrimp farming is the best business and has been a great growing, but the feed is consider the higher cost of production and the major source of pollution of shrimp farms. In this context it is need look for a feed with quality and a new ingredient. The aim of the present study was to analysis different commercial feed and another elaborate feed about the physical and chemical stability. We performed the study for 50 days. We used 35 tanks and the density was of five shrimp per aquarium. The shrimp had a feed different. The physic-chemical parameters were monitoring. We observed the weight gain of shrimp growth rates, growth rate and specific growth rate. It was also observed in lleaching of nutrients at time intervals, 04, 08 and 12 hours. The proximate food composition in feed analyses has required the requirements nutritional. The survival rate during cultivation was 74 to 88%, where shrimp fed the diet R6 had the highest growth rates. The physical stability of the diets, R1 to R7, showed significant differences between them, ranging from 34 to 141 minutes for its degradation. As the nutrient loss was gradual, with the highest was evident with the R4. The thermo gravimetric profile of the diets, R1 to R7, had similar characteristics, indicating three stages of thermal decomposition. / A Aqüicultura desenvolveu-se rapidamente nos últimos anos, sendo a carcinicultura um dos segmentos mais lucrativos e crescentes, onde a ração representa o custo mais elevado da produção e a maior fonte de poluição das fazendas de camarão. Nesse contexto, verifica-se a busca por rações de qualidade e novos ingredientes. Assim, o presente trabalho objetivou analisar diferentes tipos de ração comercial e elaborada, em seu aspecto de Estabilidade Física e Química. Realizou-se um experimento avaliando o crescimento em peso dos camarões juvenis por um período de 50 dias, utilizando 35 aquários com uma densidade populacional de 25 camarões/m2, ofertando diferentes rações comerciais e elaborada, bem como a realização do monitoramento dos parâmetros físico-químicos das águas dos cultivos, onde foram observado o ganho de peso dos camarões, a taxa de crescimento, a velocidade de crescimento e a taxa de crescimento específico. Enfim, foi verificada a lixiviação dos nutrientes em intervalos de tempo, 04, 08 e 12 horas, e a composição centesimal das rações sob a ótica das exigências nutricionais. A taxa de sobrevivência durante o cultivo foi de 74 a 88%, onde os camarões alimentados com a ração R6 apresentaram as maiores taxas de crescimento. A estabilidade física das rações, R1 a R7, apresentaram diferenças significativas entre si, variando de 34 a 141 minutos para a sua degradação. Quanto à perda de nutrientes, detectou-se prejuízo gradativo, sendo mais evidente na ração R4. Quanto ao perfil termogravimétrico das rações, todas apresentaram características semelhantes, indicando três etapas de decomposição térmica.

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