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Rheological properties of biodegradable thermosensitive copolymers
Chamradová, Ivana ; Poláček, Petr (referee) ; Vojtová, Lucy (advisor)
Hlavním cílem předložené diplomové práce byla příprava, charakterizace a reologická studie "inteligentních" injektovatelných hydrogelů, které jsou biodegradovatelné, biokompatibilní a s řízenou životností sestávajících se z hydrofilního polyethylenglykolu (PEG) a hydrofobního kopolymeru kyseliny polymléčné a polyglykolové (PLA/PGA). Výsledný termosenzitivní PLGA–PEG–PLGA kopolymer, který geluje při teplotě lidského těla, byl dále funkcionalizován anhydridem kyseliny itakonové získané z obnovitelných zdrojů, přinášející jak reaktivní dvojné vazby tak i funkční –COOH skupiny na konce kopolymeru. Navíc byl PLGA–PEG–PLGA kopolymer modifikován bioaktivním anorganickým hydroxyapatitem pro použití jako injektovatelné kostní adhezivum. Oba modifikované kopolymery jak ITA/PLGA–PEG–PLGA/ITA tak i PLGA–PEG–PLGA/HAp ovlivňují reologické vlastnosti původního PLGA—PEG—PLGA kopolymeru rozhodující o tom, zda by mohly být nové polymerní materiály vhodné jako injektovatelné nosiče léčiv nebo kostní lepidla v lékařských aplikacích. Experimentální část této práce je zaměřena především na charakterizaci viskoelastických vlastností jak nemodifikovaného PLGA—PEG—PLGA kopolymeru tak i s přidáním ITA nebo HAp metodou obrácených testovacích vialek (TTIM) a dynamickou reologickou analýzou. Výhodou TTIM je vizualizace přechodu sol-gel, určení kritické gelační teploty a kritické gelační koncentrace. Reologická měření poskytují informace o viskozitě a vizkoelasticitě gelu změnou elastického (G´) a ztrátového (G´´) modulu. Připravené kopolymery byly také charakterizovány 1H NMR a GPC. Povrch a velikost částic HAp byl popsán pomocí SEM a laserového analyzátoru částic. Původní PLGA—PEG—PLGA kopolymer i kopolymer modifikovaný ITA a HAp vykazovaly sol-gel přechod vyvolaný zvýšením teploty. Reologické vlastnosti kopolymerů v koncentračním rozmezí 6 až 24 hm. % ve vodě byly studovány buď TTIM nebo užitím reometru a získané výsledky spolu velmi dobře korespondovaly. Reologické vyhodnocení prokázalo dvě „překřížení“, kde G´ =G´´. První překřížení velmi dobře korespondovalo s prvním sol-gel přechodem nalezeným prostřednictvím TTIM. Maximální hodnota G´ odpovídající nejvyšší tuhosti polymerního gelu byla situována v bílém gelu. Druhý fázový přechod představuje přechod mezi gelem a suspenzí, kdy je bílý polymer oddělen od vody. Tuhost gelu roste s rostoucí koncentrací polymeru ve vodě. Pro srovnání, kopolymer modifikován jak ITA, tak i přidáním HAp (0, 10, 20, 30, 40, 50 hm %) vykázal zvýšení tuhosti gelu oproti původnímu kopolymeru PLGA–PEG–PLGA a přiblížení teploty maximální hodnoty G´ tělesné teplotě (37 °C). Bylo prokázáno, že jak ITA/PLGA–PEG–PLGA/ITA kopolymer tak i PLGA—PEG—PLGA/HAp kompozit jsou vhodnými kandidáty na injekovatelné systémy pro řízené uvolňování léčiv či kostní adhezivum pro ortopedii nebo zubní aplikace.
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New methods of protonated aminoacids preparation and their interactions with polyelectrolytes
Trojan, Martin ; Sedlařík,, Vladimír (referee) ; Chytil, Martin (advisor)
This Master thesis investigates the interaction between the polysaccharide sodium hyaluronate (HA) and some amphiphilic molecules. It is known that the presence of the carboxylic group on HA and the aminogroup on the amphiphiles leads to electrostatic interaction between these two compounds. This supposal offers the possibility to physically modify HA and use it as a new type of a carrier of bioactive compounds, for example medicals. However, successful carrier of bioactive compound has to resist a certain value of ionic strength. The high-molecular weights HA (1.75MDa) and amphiphile lysine were chosen for the study of the influence of ionic strength on the system HA – amphiphile. Our results show that system HA – amphiphile system is suppressed even by low concentrate solution of electrolyte. Therefore the system was reinforced by protonation of the aminoacid. The results show, that the interactions were reinforced, nevertheless negative influence of chlorine anions had to be eliminated by lyophilization. The solutions with strengthened system HA – amphiphile were used for the research of ionic strength influence. The amphiphiles lysine, 6 - aminocaproic acid and arginine were selected for this study. The interactions were investigated by means of reometry and conductometry.
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Microrheology in study of biopolmer colloids.
Hnyluchová, Zuzana ; Sedláček, Petr (referee) ; Mravec, Filip (advisor)
A new method for determining the viscoelastic properties of materials was introduced and investigated. Results of three groups of samples obtained using one particle microrheology method, DLS microrheology method and classical rheology method were compared to be sure of correctness of measurements. As a model system were chosen mixtures of glycerol of different viscosities. In case of samples containing glycerol, results were also compared with tabulated values. Hyaluronan of various molecular weights was used as a biopolymer and polystyrene particles were used for microrheology. It was confirmed, that viscosity values of biopolymer samples obtaining by each method are comparable.
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Study of emulsion stability by means of physical-chemical and optical methods
Kuchyňová, Jitka ; Veselá, Mária (referee) ; Zmeškal, Oldřich (advisor)
The diploma thesis deals with the stability determination of model O/W (30/70) emulsions at 25°C. In fact, the time and emulsifier concentration (Tego Care PS) dependences of physical properties (aging) were monitored. In the second part of the work, the influence of conservant on emulsion stabilities were studied. In order to study physical properties of emusions rheometry, differential scanning calorimetry (DSC) and optical microscopy were employed. The rheological measurement provided information on viscosity and viscoelastic modulus. DSC experiments used the repeated freezing/thawing cycles which allowed monitoring of changes in crystallization temperature of water present in emulsions and melting enthalpy of ice formed during the cooling. The optical microscopy was used to examine the change in oil droplet size in the course of emulsion destabilization and phase separation. In this case the image analysis was carried out using program HarFA. The results showed that due to the emulsion creaming, the oil droplets diffuse and aggregate which causes phase separation. Those processes were quickest for the emulsion with lowest emulsifier concentration 0.1 % (destabilization during 51 days) The emulsions with emulsifier concentration about 1.5 and 1.3 % were stable at least for 4 months. The presence of the coemulsifiers increased the elastic modulus and descreased the phase difference due to the network formation. It was shown that for the stability determination is necessary to use conservant due to risk of microbial contamination. DSC experiments allowed to distingush samples prepared under different conditions. Lower rotational speed during emulsion preparation caused the appearance of two melting and crystalization peaks while for higher speed only one peak was observed.
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Influence of selected active compounds for properties of gel and emulsion cosmetics
Gardoňová, Lenka ; Pekař, Miloslav (referee) ; Zemanová, Jana (advisor)
This master‘s thesis studies problems of chosen active substances in cosmetic emulsions and gels. There is their main characteristics – distribution and properties of cosmetic emulsions and gels, preparation of the active substances, effects on the skin and conditions, which could them influence. In experimental part, preparation of gels and emulsions bases was described which were than enriched by active substances - evening primrose oil, hemp oil, Salvia officinalis extract, Symphytum officinale extract and sea salt. Properties of these cosmetic gels and emulsions bases with the addition of active substances depend on temperature and method of storage, amount of light exposure, method of preparation and another conditions. Action of these factors can cause changes of the stability, thereby the cosmetics effects on the skin can be lost. On the bases of performed rheology measurements (oscillation and flow measurements), pH measurements and sensory analysis were determined, if the properties of examined samples were changed. The measurement was performed in the certain time intervals and the properties were evaluated like at laboratory temperature 23±2 °C, so after exposure to temperature regime 37 °C in thermoregulator. On the basis of performed measurements, there was determined, that gel base with addition of Symphytum officinale extract had the most stability properties.
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Rheological properties of gels for Pechini syntheses
Wirthová, Michaela ; Ptáček, Petr (referee) ; Zmrzlý, Martin (advisor)
This work deals with preparation of layers of ceramic materials – perovskites. The introductory part includes general characteristics concerning structure, properties and use of this materials. In details then there is described method of their preparation, namely Pechini´s syntheses, which are most widely used. Optimum molar ratio of components is discussed, in the sense of what compositions lead to creation of perovskite structures. Influence of this parameter on rheological properties of precursory gels is described in the end of the first part of work. In experimental section there are described preparations of gels, which are prepared via reaction between citric acid and ethylene glycol and gels, which are prepared by Pechini´s synthesis. Rheological properties of prepared gels (density, viscosity and surface tension) and besides determination of amount of nitrates in gels are characterized. Temperature dependence of viscosity of gels, that are prepared by reaction of citric acid and ethylene glycol are determined. In final part successful preparations of perovskite layers is shown on ceramic substrate. This layers are observed by means of light optical microscope and scanning electron microscope.
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Modification of medical hyaluronan hydrogels
Kubalová, Barbora ; Sedláček, Petr (referee) ; Venerová, Tereza (advisor)
The aim of this bachelor´s thesis was to modify the physically cross-linked hyaluronan hydrogels based on polymer-surfactant systems in order to possibly utilize them in the medical applications. Due to their antibacterial properties and viscoelasticity they are characterized as the perspective systems which can find their applications in medicine. The diversification was based on the replacement of the hyaluronan polymer networks for other polymers. Two polymers were selected for these purposes: polymer 1 and polymer 2. x% solution formed from two polymers was prepared carrying the specific amount of hyaluronan in the polymer blend of a %, b %, c %, d % and e %. The samples containing the x% system of mixed polymers which carried the specific amount of hyaluronan (e %) were measured and a surfactant solubilization ability of the hydrophilic dye Sudan red G was determined in order to confirm the physical crosslinking of the hydrogel, and the frequency rheological tests were also performed.
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Interactions of aminoclays with natural polyelectrolytes
Jančík Procházková, Anna ; Mravec, Filip (referee) ; Pekař, Miloslav (advisor)
This thesis deals with the preparation of products of interactions of aminoclay with natural polyelectrolytes. Sodium hyaluronate was chosen as the natural polyelectrolyte. The concentration and volume ratio of solutions of aminoclay and natural polyelectrolyte which led to the formation of any type of product were studied. The resulting coagulates were characterized by microscopy, FTIR spectroscopy and rheology. Furthermore the possibility of interactions with fluorescent probes was studied.
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Polysaccharide-protein gels
Hájovská, Pavla ; Smilek, Jiří (referee) ; Chytil, Martin (advisor)
This bachelor thesis deals with gelation of albumin solutions and mixed solutions of albumin and the high molecular weight hyaluronic acid due to heating. Study was carried out by measuring rheological properties of the solutions, formed gels and gelation process. For the protein samples in water, the effect of concentration, ionic strength and pH were tested. For mixed solutions, the effect of concentration and a composition of the polymeric component were tested. With increasing concentration of the polymeric component, the gel point is shifted towards lower temperature values, with the concentration difference of 2 % (w/v) up to 5°C. The resulting gels exhibit higher values of loss and storage moduli. Similar behavior was observed also in the samples influenced by the ionic strength as, a result of alternation of the electrostatic interactions between the charged groups of the polymer chains and as a result of change of this charge due to the pH reduced below the pI value of the protein.
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Rheology of collagen hydrogels and its nanocomposites
Voldánová, Michaela ; Vojtová, Lucy (referee) ; Jančář, Josef (advisor)
This bachelor thesis deals with the phenomenological description of the rheological behavior of pure collagen I and its nanocomposites with addition of hydroxyapatite in four concentrations. Measurements were performed on a rheometer in the configuration cone – plate for a range of shear rates from 0 s-1 to 100 s-1 under defined conditions. At 4 °C, the collagen in samples of a specific composition remains dissolved; collagen retains his native character and the precursors of hydrogel are in the liquid state. By heating the aqueous solution of collagen with neutral pH leeds to spontaneous crosslinking process into fibrillar structure. At 37 °C, fibrils grow into the gel structure, however, the rate of its formation is dependent on the amount of collagen fibers. The measured data are processed in the form of flow and viscosity curves, from which the rheological behavior of the sample or structural and transformational changes in response to mechanical stress and temperature changes are evaluated and compared. This knowledge can be used to manipulate with hydrogels. Generally, it can help as a basis for further development of collagen, its interaction with HAP and factors influencing their stability or effectiveness.
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