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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.
91

Suco de banana em pó probiótico / Probiotic powder banana juice

Lima, Diana Clara Nunes de, 1987- 22 August 2018 (has links)
Orientador: Flávio Luís Schmidt / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-22T03:48:15Z (GMT). No. of bitstreams: 1 Lima_DianaClaraNunesde_M.pdf: 1229443 bytes, checksum: 3bcfa21ba3ebf6795172191e5d5be6df (MD5) Previous issue date: 2013 / Resumo: O consumo de frutas vem crescendo no mercado nacional e internacional, o que está relacionado ao sabor, às preferências pessoais e com mudanças no comportamento do consumidor, que se preocupa cada vez mais com a saúde, o que promove um aumento na demanda de produtos naturais, de alto valor nutritivo. Um grupo de alimentos que também vem ganhando mercado no Brasil são os alimentos probióticos. O leite é a principal matriz alimentícia utilizada como veículo para estes micro-organismos e o desenvolvimento de alimentos probióticos de origem não láctea é uma opção atrativa diante do crescente número de consumidores vegetarianos, da intolerância à lactose, e do colesterol presente nos laticínios. Este trabalho teve o objetivo de desenvolver um suco de banana em pó e utilizá-lo como veículo para o micro-organimo probiótico Lactobacillus acidophilus. Uma mistura de purê de banana, maltodextrina, antiumectante e solução de L. acidophilus foi liofilizada, triturada e armazenada por 90 dias a 5, 25 e 35° C. A viabilidade do micro-organismo foi acompanhada durante a vida de prateleira a cada sete dias. Realizou-se também determinação da atividade de água, umidade, pH, acidez, açúcares totais e redutores e ácido ascórbico a fim de entender as relações entre a sobrevivência do L. acidophilus e os parâmetros físico-químicos do produto. Realizou-se testes in vitro a fim de verificar a tolerância do micro-organismo frente à simulação gastro-intestinal, no tempo zero (após a liofilização) e com 90 dias de armazenamento a 5° C. Além disso, fez-se a caracterização das propriedades físicas do suco em pó e das características físico-químicas do purê de banana utilizado. Na temperatura de armazenamento de 5° C as contagens mantiveram-se na ordem de 106 UFC.mL-1, não havendo diferença significativa (p>0,05) a partir do 14° dia de prateleira. Enquanto a 25 e 35° C a viabilidade reduziu gradualmente e após os 90 dias de armazenamento as contagens foram de 102 UFC.mL-1. Dentre os parâmetros físico-químicos, a atividade de água e umidade foram os que mais influenciaram na sobrevivência da cultura probiótica. O L. acidophilus demonstrou menor resistência à simulação gastro-intestinal depois dos 90 dias de armazenamento, apresentando 48% de sobrevivência. Em relação à caracterização das propriedades físicas e físico-químicas do suco em pó e do purê de banana, os resultados mostram que os produtos apresentaram características similares e qualidade compatível com a de frutas em pó produzidas por outros tipos de secadores e de polpas de frutas estudadas em trabalhos anteriores. Os resultados demonstraram que a aplicação de L. acidophilus em suco em pó de banana é viável, se o produto for armazenado a 5° C, sendo esta a temperatura que mais favoreceu a sobrevivência do probiótico e a manutenção das características físicas e químicas do suco em pó. A tolerância do L. acidophilus ao estresse gastro-intestinal diminui com o tempo de armazenamento. Quanto à caracterização do pó e do purê, os resultados atestam a qualidade do produto, se o mesmo for armazenado em embalagens adequadas e a baixas temperaturas / Abstract: The consumption of fruit is growing in the national and international market, which is related to taste, personal preferences and changes in consumer behavior that is concerned more with health, and this fact promotes an increase in demand for natural products, of high nutritional value. One food group that also has been gaining market in Brazil are the probiotic foods. Milk is the main food matrix used as a vehicle for these microorganisms and the development of probiotic foods of non dairy origin is an attractive option because of its increasing number of vegetarians consumers, lactose intolerance, and the cholesterol content in dairy products. This study aimed to develop a banana puree powder and its use as a vehicle for the probiotic microorganism Lactobacillus acidophilus. A mixture of banana pulp, maltodextrin, antiwetting agent and solution of L. acidophilus was freeze-dried, crushed and stored for 90 days at 5, 25 and 35 °C. The viability of this microorganism was accompanied during the shelf life study measuring also water activity, moisture, pH, acidity, total and reducing sugars and ascorbic acid in order to understand the relationship between survival of L. acidophilus and physico-chemical parameters of the product. It was conducted in vitro tests to verify the tolerance of the microorganism in the gastro-intestinal simulation, at time zero (after freeze dried) and 90 days storage at 5 ° C. Moreover, it was the characterization of physical properties of powdered juice and physicochemical characteristics of banana puree used. At the storage temperature of 5 ° C counts remained in the order of 106 UFC.mL-1, with no significant difference (p> 0.05) from day 14 of the shelf life. While 25 and 35 ° C the viability decreased gradually and after 90 days of storage counts were 102 UFC.mL-1. Among the physico-chemical parameters, water activity and moisture were most influenced the survival of probiotic culture. L. acidophilus showed less resistance to simulated gastro-intestinal tract after 90 days of storage, showing 48% survival. With respect to the characterization of physical and physical-chemical properties of powdered juice and banana puree, the results showed that the products have similar characteristics and quality compatible with fruit powder produced by other types of dryers and fruit pulp studied in previous works. It was concluded, that the application of L. acidophilus in banana juice powder is viable if the product is stored at 5 °C, this being the temperature at which most favored the survival of the probiotic and maintenance of the physical and chemical characteristics of the juice powder. The tolerance of L. acidophilus to gastro-intestinal stress decreases with the time. As for powder characterization and puree, results substantiate the quality of the product, whether it is stored in appropriate packaging and low temperatures / Mestrado / Tecnologia de Alimentos / Mestra em Tecnologia de Alimentos
92

Vliv biologicky aktivních látek na strukturu a vlastnosti kolagenových substrátů / The effect of biologicaly active substances on the structure and properties of collagenous substrates

Muchová, Johana January 2016 (has links)
Diplomová práce se zabývá přípravou 3D porézních kolagenových skafoldů metodou lyofilizace a jejich modifikací bioaktivními látkami. K modifikaci byly použity přírodní polysacharidy – chitosan, vápenatá oxidovaná celulóza a chitin/chitosan-glukanový komplex. Mechanické vlastnosti skafoldů byly upraveny síťováním pomocí karbodiimidů. Růstové faktory byly dodány formou destičkového lyzátu. Byl zkoumán vliv biologicky aktivních aditiv, siťovacího činidla a obohacení růstovými faktory na vlastnosti připravených skaffoldů a jejich bioaktivitu v tkáních živých organismů. Konkrétně byly studovány morfologické vlastnosti, struktura, porozita, botnání, stabilita, chemické složení, teplota denaturace a biologické vlastnosti. K charakterizaci byly použity metody rastrovací elektronová mikroskopie, infračervená spektroskopie, diferenční kompenzační kalorimetrie a konfokální mikroskop. Připravené kolagenové substráty obohaceny bioaktivním aditivem a destičkovým lyzátem mohou být využity v biomedicíně jako skafoldy pro růst buněk v systémech s nízkou mechanickou zátěží.
93

Obtenção de compostos fenólicos em pó por liofilização a partir da torta residual de pequi /

Nunes, Natalie Stephanie Sawada January 2020 (has links)
Orientador: Cassia Roberta Malacrida Mayer / Resumo: O Cerrado, segundo maior bioma brasileiro, possui uma rica flora e fauna dentre as savanas do mundo. O pequi (Caryocar brasiliense Camb.) é um fruto nativo desse bioma e apresenta muitos compostos bioativos como carotenoides, vitaminas A e E e compostos fenólicos que possuem ações anticarcinogênicas, antimicrobianas e antioxidantes. Esses compostos, no entanto, são sensíveis a exposição à luz e oxigênio. Para amenizar essa degradação podem ser utilizados métodos de encapsulação. A extração do óleo da polpa de pequi, por prensagem a frio, gera uma torta residual rica em compostos bioativos. Portanto, o objetivo do presente trabalho foi a encapsulação dos compostos fenólicos presentes na torta residual por meio da liofilização utilizando diferentes agentes encapsulantes (amido de mandioca modificado, goma arábica, maltodextrina e ovoalbumina). Para tanto foi obtido um extrato aquoso (1:6 m/v) da torta residual utilizando extração ultrassônica com os seguintes parâmetros: 240 W de potência, 50% de pulso e 10 minutos. Os materiais encapsulantes corresponderam a 20% do extrato. Inicialmente, o extrato foi misturado aos agentes encapsulantes puros com o intuito de verificar quais os melhores encapsulantes. Numa segunda etapa, foram utilizadas misturas de amido de mandioca modificado (AM) e maltodextrina (MD) para misturas nas proporções de 50% de AM e 50% de MD; 75% AM e 25% MD e 25% AM e 75% MD. Todas as amostras foram liofilizadas a -50 °C por 48 horas, originando pós de cor amar... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The Cerrado, the second largest Brazilian biome, has a rich flora and fauna among the world’s savannas. Pequi (Caryocar Brasiliense Camb.) is a native fruit of this biome and has several bioactive compounds such as carotenoids, vitamins A and E and phenolic compounds that perform anticarcinogenic, antimicrobial and antioxidants actions. These compounds, however, are sensitive to light and oxygen exposure. To mitigate this degradation, encapsulation methods can be used. The oil extraction from pequi pulp, by cold pressing, generates a residual cake rich in bioactive compounds. Therefore, the objective of the present work was the encapsulation of the phenolic compounds present in the residual cake by freeze-drying using different encapsulating agents (modified cassava starch, Arabic gum, maltodextrin and ovoalbumin). For this, an aqueous extract (1:6 m/v) of the residual cake was obtained using ultrasonic extraction with the following parameters: 240 W of power, 50% of pulse and 10 minutes. The encapsulating materials corresponded to 20% of the extract. Initially, the extract was mixed with pure encapsulating in order to verify which are the best encapsulating. In second stage, modified cassava starch (AM) and maltodextrin (MD) were used for mixtures in the proportions of 50% AM and 50% MD; 75% AM and 25 MD and 25% AM and 75% MD. All samples were freezing drying at -50°C for 48 hours, resulting in yellowish powders, which were evaluated for physicochemical characteristics. Afte... (Complete abstract click electronic access below) / Mestre
94

IoT Sensors for Industrial and Agricultural Applications: Development of Wireless Network and Process Control

Xiaofan Jiang (9755084) 14 December 2020 (has links)
As the new paradigm of data collection enabled by the advancements in wireless technology and digital electronics, small sensing devices have started to be used in everyday life. These devices are capable of sensing, computing, communicating, and forming a wireless sensor network (WSN) which is necessary to provide sensing services and to monitor various conditions. In addition to WSNs, the idea of Internet of Things (IoT) has started to draw more attention. IoT is defined as an interconnection between identifiable devices within the internet for sensing and monitoring processes. This dissertation addresses the development of wireless network and process control for two challenging IoT applications, namely smart agriculture and industrial lyophilization.<div><br><div>Smart agriculture refers to the concept of using modern technology to increase the quantity and quality of agricultural products. This dissertation presents a novel hybrid large-area IoT network by combining the low-power wide-area network (LPWAN) as well as ultra-low-power wireless personal area networks (WPAN) that delivers wide-area coverage while maintaining low-power operation. </div><div><br></div><div>Lyophilization is the process of removing water content from a material with the objective of increasing its stability and, hence, its shelf life. Continuous inline process tracking is imperative to a successful lyophilization process in industrial pharmaceuticals. To address this need, this dissertation presents two wireless sensing systems that are capable of monitoring lyophilization process with detailed design and demonstration<br></div></div>
95

Developing Production Methods for Different Microbial Strains and Beneficial Testing on Crop Species

Alghanmi, Linah Y. 07 1900 (has links)
Microorganisms will play a significant role in the agricultural revolution in the coming decades and help meet the growing population's needs. Hence, understanding the impact of beneficial bacteria on crop development is key to the future of developing microbial products. The ability of PGPB to increase crop yields has been recently investigated in agriculture, as PGPB can support and protect plants under different stresses. Since PGPB interactions occur naturally, finding a method to apply beneficial bacteria while maintaining their efficiency and quality is a topic of interest. PGPB have been used as microbial inoculants, biofertilizers, and also as seed coatings. Preservation of microorganisms through desiccation has been used as the preferred method for long-term storage of microbial culture. The use of dry powders is favored over liquid cultures due to their ease of transportation and better quality control. For microbial preservation, freeze-drying has been defined as the most convenient and satisfactory preservation method for long-term storage. Freeze-drying is generally preferred over other drying techniques as it gives a high-quality dehydrated product. However, to reach a high-quality product, many parameters need to be monitored, such as bacterial cell concentration, growth medium, lyophilization buffer, rehydration, and duration of freeze-drying. In this research, SA190 was freeze-dried with 10% sucrose mixed with 5% trehalose as lyophilization buffer. Pseudomonas argentinensis SA190 was isolated from the root nodules of the desert plant Indigofera argentae in Saudi Arabia, specifically Jizan. The SA190 freeze-dried product was examined by several tests to assess the product viability and quality, such as accelerated test and water stability test. For future work, the effect of freeze-dried SA190 on plant growth and crop yield will be investigated. Moreover, optimization of the freeze-drying process, formulation, and packaging for commercial will be considered. In addition, bacterial strains isolated in DARWIN21 project with promising effects on plant growth, will be subjected to freeze-drying process.
96

Influence of Stress Treatments on the Resistance of <em>Lactococcus lactis</em> to Freezing and Freeze-Drying

Lin, Chan 01 May 1998 (has links)
This study investigated the effect of cold, heat, or osmotic shock treatment on the resistance of L. lactis subsp. cremoris MM160 and MM310 and Lactococcus lactis subsp. lactis MM210 and FG2 cheese starter bacteria to freezing and freeze-drying. The ability to withstand freezing at -60°C for 24 h was variable among lactococci, but resistance to this treatment was significantly improved (P < 0.05) in most strains by a 2-h cold shock at l0°C or a 25-min heat shock at 39°C (L. lactis subsp. cremoris) or 42°C (L. lactis subsp. lactis). Stress treatments that improved lactococcal freeze resistance were also found to significantly (P < 0.05) enhance the resistance of most strains to lyophilization. Increased resistance to freezing or lyophilization was not detected when stress treatments were performed in broth that contained erythromycin, which indicated stress-inducible proteins were involved in cell protection. Membrane fatty acid analysis of stress-treated cells suggested that enhanced resistance to freezing and lyophilization may be related to heat or cold shock-induced changes in cell membrane composition. Heat-shocked cells had a higher 19:0 cyclopropane fatty acid content than did control cells, and cold-shocked cells contained a lower ratio of saturated to unsaturated fatty acids. Other factors must also be involved in cell protection, however, because similar changes in membrane composition were also detected in strains whose resistance to freezing and lyophilization was not improved by heat or cold shock.
97

EFFECTS OF FORMULATION COMPONENTS AND DRYING TECHNIQUES ON STRUCTURE AND PHYSICAL STABILITY OF PROTEIN FORMULATIONS

Tarun Tejasvi Mutukuri (11581819) 22 April 2022 (has links)
<p>  </p> <p>With the recent growth in demand for biologics across the globe, it remains critical to manufacture these biologics in solid-state to improve stability as well as to increase the ease of transportation across the world. To meet these increased demands, it is of paramount importance to use various processing methods that have shorter processing times. It is also important to understand the impact of the processing methods and various formulation components on the stability of the proteins.  In Chapter 1, a review of the various processing methods that are used in the industry along with additional processing methods that are being investigated will be discussed. The common drying methods such as lyophilization and spray drying along with the novel techniques as well as specific examples of processing parameters to improve the processing conditions that better suit the protein formulations will be mentioned. </p> <p>The studies in Chapter 2 examined the effects of processing methods (freeze drying and spray freeze drying) and the excipients on the protein structure and physical stability. Protein solids containing one of two model proteins (lysozyme or myoglobin) were produced with or without excipients (sucrose or mannitol) using freeze drying or spray freeze drying (SFD). The protein powders were then characterized using solid-state Fourier transform infrared spectroscopy (ssFTIR), differential scanning calorimetry (DSC), circular dichroism spectrometry (CD), size exclusion chromatography (SEC), BET surface area measurements, and solid-state hydrogen-deuterium exchange with mass spectrometry (ssHDX-MS). ssFTIR and CD could identify little to no difference in the structure of the proteins in the formulation. ssHDX-MS was able to identify the population heterogeneity, which was undetectable by conventional characterization techniques of ssFTIR and CD. ssHDX-MS metrics such as Dmax and peak area showed a good correlation with the protein physical instability (loss of the monomeric peak area by size exclusion chromatography) in 90-day stability studies conducted at 40oC for lysozyme.  The higher specific surface area was associated with greater loss in monomer content for myoglobin-mannitol formulations as compared to myoglobin-only formulations. Spray freeze drying seems a viable manufacturing technique for protein solids with appropriate optimization of formulations. The differences observed within the formulations and between the processes using ssHDX-MS, BET surface area measurements, and SEC in this study provide an insight into the influence of drying methods and excipients on protein physical stability.</p> <p>Based on this work, it was identified that spray freeze drying can be a viable alternative to produce solid-state protein formulations with similar stability as the freeze drying process. However, due to the long processing times and scale-up issues involved in the spray freeze drying process, there is a necessity to explore additional drying processes. Chapter 3 focuses on using another novel technique known as electrostatic spray drying (ESD) to produce solid-state protein formulations at lower drying temperatures than conventional spray drying and its effect on protein stability. A mAb formulation was dried by either conventional spray drying or electrostatic spray drying with charge (ESD). The protein powders were then characterized using solid-state Fourier transform infrared spectroscopy (ssFTIR), differential scanning calorimetry (DSC), size exclusion chromatography (SEC), and solid-state hydrogen/deuterium exchange with mass spectrometry (ssHDX-MS). Particle characterizations such as BET surface area, particle size distribution, and particle morphology were also performed. Conventional spray drying of the mAb formulation at the inlet temperature of 70oC failed to generate dry powders due to poor drying efficiency; electrostatic spray drying at the same temperature at 5kV enabled the formation of powder formulation with satisfactory moisture contents. Deconvoluted peak areas of deuterated samples from the ssHDX-MS study showed a good correlation with the loss of the monomeric peak area measured by size exclusion chromatography in the 90-day accelerated stability study conducted at 40oC. Low-temperature (70oC inlet temperature) drying with an electrostatic charge (5kV) led to better protein physical stability as compared with the samples spray-dried at the high temperature (130oC inlet temperature) without charge.</p> <p>This study shows that electrostatic spray drying can produce solid monoclonal antibody formulation at a lower inlet temperature than traditional spray drying with better physical stability. While ESD can be a viable option for thermal-sensitive formulations, it is important to understand the impact of various formulation components on the stability of the proteins while using spray drying. Based on our previous studies, a good understanding of the effect of different sugars and the presence of surfactants on the spray-dried proteins has been established. However, the impact of the selection of buffer on protein stability has not been studied. In Chapter 4, the effect of buffer salts on the physical stability of spray dried and lyophilized formulations of a model protein, bovine serum albumin (BSA) were examined. BSA formulations with various buffers were dried by either lyophilization or spray drying. The protein powders were then characterized using solid-state Fourier transform infrared spectroscopy (ssFTIR), powder X-ray diffraction (PXRD), size exclusion chromatography (SEC), solid-state hydrogen/deuterium exchange with mass spectrometry (ssHDX-MS), and solid-state nuclear magnetic resonance spectroscopy (ssNMR). Particle characterizations such as BET surface area, particle size distribution, and particle morphology were also performed. Results from conventional techniques such as ssFTIR did not exhibit correlations with the physical stability of studied formulations. Deconvoluted peak areas of deuterated samples from the ssHDX-MS study showed a satisfactory correlation with the loss of the monomeric peak area measured by SEC (R2 of 0.8722 for spray-dried formulations and 0.8428 for lyophilized formulations) in the 90-day accelerated stability study conducted at 40oC. PXRD was unable to measure phase separation in the samples right after drying. In contrast, ssNMR successfully detected the occurrence of phase separation between the succinic buffer component and protein in the lyophilized formulation, which results in a distribution of microenvironmental acidity and the subsequent loss of long-term stability. In summary, this study demonstrated that buffer salts have less impact on physical stability for the spray-dried formulations than the lyophilized solids.</p> <p>The study in Chapter 5 looked at examining the physical stability of spray freeze dried (SFD) bovine serum albumin (BSA) solids produced using the radio frequency (RF)-assisted drying technique. BSA formulations were prepared with varying concentrations of trehalose and mannitol, with an excipient-free formulation as control. These formulations were produced using traditional spray freeze drying (SFD) or RF-assisted spray freeze drying (RFSFD). The dried formulations were then characterized using solid-state Fourier transform infrared spectroscopy (ssFTIR), Karl Fischer moisture content measurement, powder X-ray diffraction (PXRD), size exclusion chromatography (SEC), solid-state hydrogen/deuterium exchange with mass spectrometry (ssHDX-MS). Traditional characterization tools such as ssFTIR and moisture content did not have a good correlation with the physical stability of the formulations measured by SEC. ssHDX-MS metrics such as the maximum deuterium uptake (Dmax) (R2 = 0.791) and deconvoluted peak areas of the deuterated samples (R2 = 0.914) showed a satisfactory correlation with the SEC stability data. RFSFD improved the stability of formulations with 20 mg/ml of trehalose and no mannitol and had similar stability with all other formulations as compared to SFD. This study demonstrated that the RFSFD technique can significantly reduce the duration of primary drying cycle from 48 h to 27.5 h while maintaining or improving protein physical stability as compared to traditional lyophilization.</p> <p>Lastly, Chapter 6 consists of a summary of the conclusions formed from the work presented in this thesis. Furthermore, suggestions for future work are provided based on observations of results, less-explored areas of formulation and processing conditions as well as characterization tools to understand effects on protein physical stability.</p> <p><br></p>
98

Pharmaceutical Nanocomposites : Structure–Mobility–Functionality Relationships in the Amorphous State

Hellrup, Joel January 2016 (has links)
Amorphous materials are found in pharmaceutical formulations both as excipients and active ingredients. Indeed, these formulations are becoming an essential strategy for incorporating drugs into well-performing solid dosage forms. However, there is an unmet need of better understanding of the microstructure and component interactions in amorphous formulations to be able to design materials with improved functionalities. The aim of this thesis is to give deepened knowledge about structure-mobility-functionality relationships in amorphous for-mulations by studying composites produced from sugars and filler particles. The structure, the mobility, and physical stability of the composite materials were studied using calorimetry, X-ray diffraction, microscopy, spectroscopy, and molecular dynamics simulations. Further, the moisture sorption of the composites was determined with dynamic vapor sorption. The compression mechanics of the composites was evaluated with compression analysis. It was demonstrated that fillers change the overall properties of the amorphous material. Specifically, the physical stability of the composite was by far improved compared to the amorphous sugar alone. This effect was pronounced for formulations with 60 wt% filler content or more. Amorphous lactose that normally recrystallizes within a few minutes upon humidity exposure, could withstand recrystallization for several months at 60% RH in composites with 80 wt% cellulose nanocrystals (CNC) or sodium montmorillonite (Na-MMT). The increased physical stability of the amorphous sugars was related to intra-particle confinement in extra-particle voids formed by the fillers and to immobilization of the amorphous phase at the surface of the fillers. Also, the composite formation led to increased particle hardness for the lactose/CNC and the lactose/Na-MMT nanocomposites. The largest effect on particle hardness was seen with 40-60 wt% nanofiller and could be related to skeleton formation of the nanofillers within the composite particles. The hygroscopicity for the lactose/Na-MMT nanocomposites decreased as much as 47% compared to ideal simple mixtures of the neat components. The nanofillers did not influence the water sorption capacity in the amorphous domains; however, lactose (intercalated into Na-MMT) interacted with the sodium ions in the interlayer space which led to the lowered hygroscopicity of this phase. The thesis advanced the knowledge of the microstructure of amorphous pharmaceutical com-posites and its relationship with pharmaceutical functionalities. It also presented new approaches for stabilizing the amorphous state by using fillers. The concept illustrated here might be used to understand similar phenomena of stabilization of amorphous formulations.
99

Photodegradation study of 3,5-diamino-6-chloro- N-(2-(methylamino)ethyl)pyrazine-2-carboxamide using preparative SFC and LC-MS

Sillén, Sara January 2016 (has links)
In this project the photodegradation of 3,5-diamino-6-chloro-N-(2-(methylamino)ethyl)pyrazine-2-carboxamide was studied. A hypothetical degradation pattern for the compound was proposed and the aim of the project was to study the formed secondary photodegradants and to, if possible, structure elucidate some of these compounds. In order to do this, the parent compound was photodegraded in two steps, where a primary photodegradant was isolated using semi-preparative supercritical fluid chromatography (SFC) and then further degraded into the secondary photodegradants. The photodegradation was first carried out in aqueous solution, where the parent compound was irradiated in UV-A light of 300-400 nm. This resulted in a primary photodegradant with a molecular ion of m/z = 227, where the chloride in position 6 of the pyrazine group had been replaced by a hydroxyl group. During the large scale photodegradation, prior to the preparative purification, the yield of primary photodegradant was very low due to the photodegradation being dependent on both sample volume and concentration and due to the primary photodegradant also being unstable in aqueous solution at room temperature. Due to the above mentioned difficulties the parent compound was photodegraded in methanol instead of water in order to avoid the freeze-drying process where a lot of the primary photodegradant was lost. This resulted in a primary photodegradant with a molecular ion of m/z = 241, where the chloride had been replaced by a methoxy group instead of a hydroxyl group. This compound was more stable which allowed workup by rotary evaporation, instead of freeze-drying, before the preparative purification. This primary photodegradant was isolated using semi-preparative SFC on a Viridis® BEH Prep OBD TM column (250 x 30 mm, 5 µm) and a Luna HILIC column (250 x 30 mm, 5 µm) with MeOH/NH3 100/1 v/v as organic modifier. About 1.2 mg material was isolated and further photodegradation tests in ordinary water and 18O-water were conducted. Some secondary photodegradants were observed in LC-MS analyses, and their element compositions were proposed by accurate mass results. Fundamental structures for these compounds were proposed. Further structural investigational analyses are needed for confirmation in the future.
100

Etude des transferts d'arômes encapsulés dans une matrice alimentaire type génoise / Study of encapsulated flavours transfers in food matrix like sponge cake

Madene, Atmane 14 November 2006 (has links)
Ces travaux portent sur l’étude du transfert de l’arôme viennoiserie encapsulé dans une matrice constituée du mélange gomme acacia – maltodextrines et incorporé dans une génoise emballée (plastiques et papier), dans des conditions contrôlées de stockage (humidité relative et température). Le procédé d’encapsulation utilisé dans cette étude est la lyophilisation. Les propriétés physicochimiques des molécules volatiles influencent leur rétention. Ainsi, les molécules hydrophobes à haut poids moléculaire sont mieux conservées dans ce système. L’incorporation de capsules d’arômes dans les génoises influence leurs propriétés physiques (la couleur et la texture) et favorise la formation d’une croûte pouvant jouer un rôle barrière sur les transferts d’arômes. Au cours du stockage des génoises emballées, l’apport positif de l’encapsulation sur la rétention des arômes a été révélé. Le type d’emballage peut influencer la perte en composés d’arôme dans l’espace de tête génoise – emballage. Ainsi, les emballages plastiques offrent une meilleure conservation des molécules volatiles par rapport aux papiers traités / This study deals with transfer of viennoiserie aroma encapsulated in a acacia gum - maltodextrines matrix and incorporated in a packaged sponge cake (plastic and treated-paper), under controlled storage conditions (temperature and relative humidity). The process of encapsulation used in this work is freeze-drying. The physicochemical properties of the volatiles molecules influence their retention in the matrix. Thus, the hydrophobic molecules with high molecular weight are more retained. The incorporation of capsules in the sponge cake matrix influences the physical properties of food matrix (color and texture) and supports the formation of a crust which acts as a barrier in the flavour transfer. It was noted that encapsulation contributed in retaining flavour compounds during the storage of packaged sponge cake. Also, the type of packaging can influence the loss of flavour in the headspace between sponge cake and packaging. Indeed, plastic packaging offers a better conservation of volatiles molecules compared to treated-papers

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