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Optimisation of polyethylene glycol hydrogels preparation by polymerisation and their subsequent characterisation
Fornůsek, Jakub ; Trudičová, Monika (referee) ; Smilek, Jiří (advisor)
The goal of this bachelor’s thesis was the optimization of the preparation of polyethyleneglycol hydrogels by radical polymerization and their subsequent characterization by the means of rheometry, swelling experiments and examination of transport properties through the absorption of an active substance and its subsequent desorption. To examine these hydrogels, UV photopolymerization was chosen due to its simplicity and reproducibility. As part of the optimalization, hydrogels were prepared under varying conditions and then characterised by the previously mentioned methods. The effect of the presence of the cross-linking agent ethylenglycol dimethacrylate on the properties of the resulting hydrogels was also investigated. These examined gels represent a new type of chemically cross-linked hydrogels, which are part of a basic research project applications by GAČR. From rheometric measurements, it was confirmed that a higher molecular weight of the measured sample corresponded to lower values of viscoelastic moduli. The effect of the cross-linking agent on these values was negligible. The mesh density played a significant role in swelling and transport experiments. As its value increased, the swelling capacity of the hydrogel decreased and therefore a smaller amount of water was absorbed. The presence of the cross-linking agent was also noticeable, as it contributed to a creation of higher density polymer networks.
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Preparation and characterisation of polysaccharide hydrogels
Kulíšková, Kateřina ; Kadlec, Martin (referee) ; Smilek, Jiří (advisor)
This bachelor thesis deals with the study of preparation and characterization of alginate hydrogels. It focuses mainly on the ionic crosslinking of alginate using divalent metal cations Ca2+, Cu2+, Zn2+, Ba2+, Fe2+ together with the trivalent cation Fe3+ in order to compare the crosslinking abilities of different oxidation states. The exogenous method was used for the preparation of alginate hydrogels and the prepared hydrogels were thus studied in the form of millimetre spheres. In the experimental part, optimization was performed to find out the optimum gelation time, which resulted in the crosslinking of the hydrogels throughout their volume. Ca2+ ions were used as a reference due to their wide application and the extensive experience with these ions at the faculty. The knowledge from the optimization was applied to the preparation of the other ions samples. The viscoelastic properties of the hydrogels were investigated by rheological measurements in the form of amplitude and squeeze tests. All ions, except Fe2+, were found to crosslink the hydrogels throughout the volume. Based on the complex modulus, the order of ions was determined according to the degree of crosslinking, The degree of crosslinking also has major impact on the degree of syneresis.
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Gel-forming substances of natural cosmetics
Prokopová, Pavla ; Smilek, Jiří (referee) ; Pekař, Miloslav (advisor)
This bachelor thesis is focused on hydrogels preparation for natural cosmetics also it focused on those prepared hydrogels. The aim of the experimental part is to specify physical and chemical properties of hydrogels prepared from commercially available polysaccharides, which agree with conditionals of natural cosmetics standards. First phase of practical part was to prepare and optimize the preparation procedure of individual hydrogels and determine their optimal concentration for use in their characterization. The second phase was the actual preparation of samples for rheometric determination. The last stage was the rheometry itself. The four raw materials selected directly from the CPK Standards were xanthan gum, guar gum, tragacanth gum and gum arabic. The results clearly demonstrated that the best raw material for the preparation of natural hydrogel is xanthan gum. On the other hand, hydrogel from gum arabic is almost impossible to prepare.
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Rheological characterization of polysaccharide gels with incorporated vesicles
Kalendová, Lucie ; Smilek, Jiří (referee) ; Venerová, Tereza (advisor)
This diploma thesis deals with the rheological characterization of polysaccharide gels with incorporated vesicular systems. Positively charged Ion Pair Amphiphile vesicles (IPA) consisting of cetrimethylammonium bromide, sodium dodecyl sulfate, dioctadecyldimethylammonium chloride and cholesterol were chosen for the incorporation. Other vesicles used for incorporation were oppositely charged liposomes made of phosphatidylcholine (DPPC), phosphatidic acid (PA) and cholesterol. The thesis is divided into two sections. The first one deals with preparation, characterization and stability control (temperature and time stability) of both vesicular systems by using dynamic light scattering (DLS). In this part, the vesicles’ stability was confirmed which made them perfect candidates for the following incorporation. The second part of the thesis describes the preparation and rheological characterization of selected gels. Three types of gels were prepared in total, specifically 1% and 2% gellan gum gels and 4% hyaluronic gel. All of them were studied in water, as well as in solutions of IPA vesicles or DPPC liposomes, both of same concentration (1 mmoll-). The subsequent rheological characterization including amplitude, frequency, and stress relaxation sweeps demonstrates there is no significant difference between reference gels and those containing vesicles. This indicates that vesicles used in this thesis were only freely stored in the gel networks, meaning the structure of the gels didn’t affect their transport properties. This is a significant information for using these systems in drug delivery.
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Transport of pharmaceuticals in model hydrogels
Horváth, Michal ; Enev, Vojtěch (referee) ; Klučáková, Martina (advisor)
This thesis was devoted to the transport properties of diclofenac in model hydrogels. Gels were prepared from agarose and some were enriched with IHSS Elliott Soil humic acid. The addition of humic acid to the hydrogel should mimic the soil environment. And it was the soil environment that was chosen to observe the transport and transfer of diclofenac. Diffusion was observed in diffusion cells, where one part contained diclofenac solution and the other MQ water. And there was a hydrogel between the cells. Samples were taken from both cells and measured spectrophotometrically at different time intervals until equilibrium was established. These measurements were finally used to describe the movement of diclofenac in the hydrogels.
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Alternative crosslinking methods for sodium alginate resulting in hydrogels with suitable application properties
Kouřilová, Ludmila ; Kráčalík, Milan (referee) ; Smilek, Jiří (advisor)
This diploma thesis is focused on the preparation of alginate gels with the potential to influence their final application properties (transparency, syneresis, viscoelastic properties, etc.). Based on literature review, a total of three gelation strategies leading to the gelation of sodium alginate were selected, namely ionotropic gelation by external gelation method, ionotropic gelation by internal gelation method, and alginate crosslinking with phytic acid, which is capable of forming both ionic bonds and intramolecular hydrogen bonds. Subsequently, the preparation of alginate gels was optimized, their mechanical properties were characterized, and finally, the influence of several factors (polymer concentration, amount of crosslinking agent, gelation time, addition of sucrose, etc.) on the resulting properties of the prepared gels was monitored. Within the scope of the thesis, it was demonstrated that the resulting properties of sodium alginate-based gels are influenced not only by the polymer concentration, the amount of crosslinking agent used, gelation rate, or syneresis, but in the case of ionotropic gelation by external gelation, for example, also by the type of anion used. An interesting part of the thesis is also the optimization of determining the mechanical properties of alginate gels through compression tests. During these tests, the sample is compressed between two rheometer sensors, and the mechanical response of sample to the applied force is measured. It is one of the most easily conceivable rheometric tests.
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Optimization of hydrogel carrier for assessment of antimicrobial activity of biocidal surfaces
Antálek, Adam ; Jančovičová, Viera (referee) ; Králová, Marcela (advisor)
This diploma thesis deals with the optimization of the composition and properties of hydrogels as carriers of microbial populations for the evaluation of the antimicrobial effects. There are standardized procedures for assessing antimicrobial surfaces, but they have shortcomings, such as the necessity of testing exclusively under laboratory conditions. In the presented work, a new evaluation methodology is proposed, which utilizes a modified resazurin test and hydrogels as platforms for bacterial seeding, enabling the assessment of the investigated antimicrobial surface. The composition and properties of hydrogel carriers were successfully optimized with respect to their swelling and mechanical properties, thereby improving recovery compared to standardized procedures. Tests on antimicrobial materials showed that the bacteria used on hydrogels continued to grow, rendering the use of composite hydrogels for this application impractical.
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Micro/macro-scale investigation of the viscoelastic properties of hydrogel materials
Obrusníková, Klára ; Pekař, Miloslav (referee) ; Smilek, Jiří (advisor)
Tato diplomová diplomová práce byla zaměřená na srovnání mezi mikroreologickými metodami a makroreologickým přístupem, zejména při charakterizaci hydrogelů. Dynamický rozptyl světla, fluorescenční korelační spektroskopie a optická pinzeta byly vybrány jako mikroreologické techniky, zatímco oscilační reometrie sloužila jako makroreologický nástroj. Výsledky z dynamického rozptylu světla a fluorescenční korelační spektroskopie pro hydrogely agarózy a gellanu byly porovnány s reometrií a mezi sebou. Hodnoty viskoelastických modulů získané z mikroreologických měření byly výrazně nižší než ty získané pomocí makroreologie. Jak dynamický rozptyl světla, tak fluorescenční korelační spektroskopie nabízejí širší škálu měřitelných frekvencí než reometrie, ale obě metody mají své limitace při charakterizaci hydrogelů. U dynamického rozptylu světla dochází k odrazu světla od gelové sítě, což způsobuje šum a zhoršuje kvalitu získaných výsledků. Fluorescenční korelační spektroskopie, přes svou vyšší specifitu, vykazuje jen velmi malé rozdíly mezi vzorky různých koncentrací. Optická pinzeta je na Fakultě chemické novou metodou, a byla provedena pouze kalibrační měření. Tuhost optické pasti, důležitá hodnota pro kalibraci optické pinzety, byla stanovena pro roztoky glycerolu.
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Effect of enzymes on the degradation of thermosensitive copolymers for controlled release of drugs
Dávidíková, Anna Mária ; Michlovská, Lenka (referee) ; Vojtová, Lucy (advisor)
Termocitlivé hydrogély, ktoré sa používajú ako nosiče liečiv v dnešnej dobe zažívajú obrovský záujem v spoločnosti. Používajú sa ako spôsob dopravy liečiva na predom určené miesto a po dosiahnutí určeného miesta slúžia ako dlhodobé úložisko liečiv v tele. Vlastnosti hydrogélov môžu byť upravované tak, aby dokázali naviazať rôzne druhy liečiv, aby boli citlivé na rôzne vonkajšie impulzy a aby degradovali pomalšie, čo predĺži životnosť liečiv v tele. Aby sme vedeli, ako upraviť vlastnosti hydrogélov a ako sa budú správať, musíme poznať ich degradačný proces a chovanie v rôznych degradačných médiách. Práve preto sú degradačné štúdie veľmi dôležitou súčasťou štúdií hydrogélov. Táto bakalárska práca je zameraná na sledovanie degradácie rôznych roztokov termocitlivého hydrogélu vo viacerých degradačných médiách. Teoretická časť práce zahrňuje krátky prehľad o tom, čo sú to termocitlivé hydrogély, ich charakterizácia a popis vlastností spolu s použitím hydrogélov ako nosičov liečiv. Ďalej sa teoretická časť venuje degradácií hydrogélov celkovo ako aj degradácií konkrétne použitého hydrogélu v tejto bakalárskej práci. V prvom rade bol syntetizovaný živou polymeráciou za otváraním kruhu v inertnej atmosfére termocitlivý PLGA-PEG-PLGA kopolymér, tvorený poly(mliečnou-co-glykolovou kyselinou)-b-poly(ethylen glykolom)-b-poly(mliečnou-co-glykolovou kyselinou). Následne bol kopolymér charakterizovaný na protónovej nukleárnej magnetickej rezonancii a na gélovej chromatografii. Z nasyntetizovaného kopolyméru boli pripravené tri vodné roztoky hydrogélu o rôznych koncentráciách a to 10, 15 a 20 hm %. Vzorky pripravených hydrogélov za teploty 37 , boli degradované v rôznych degradačných roztokoch (UPW (ultra čistá voda), NaCl, PBS (fosfátový pufr) a roztok PBS s enzýmom). Degradačná štúdia bola hlavným cieľom tejto bakalárskej práce. Jednotlivé vzorky boli odobrané v konkrétne stanovené časy a to po 1, 2, 3, 7, 9, 14, 16, 21, 23 a 30 dňoch. Pri vzorkách s enzýmom bola predpokladaná rýchlejšia degradácia vzoriek, tak tieto odbery boli nastavené po 1, 2 a 3 dňoch. Ďalším cieľom tejto práce bola analýza odobraných vzoriek hydrogélov po degradácií na gélovej chromatografii a analýza degradačných médií na kvapalinovej chromatografií s hmotnostným spektrometrom. Počas degradácie vzoriek bola prevedená taktiež gravimetrická analýza a pri odoberaní degradačných roztokov bolo merané ich pH. Následne boli všetky získané dáta vyhodnotené a bolo sledované, či enzým urýchľuje PLGA-PEG-PLGA hydrolytickú degradačnú kinetiku. Výsledky poukazujú na to, že enzým má nízky vplyv na rýchlosť degradácie. Výsledky tejto práce poslúžia ako základy pre budúce degradačné štúdie.
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Application of microencapsulation techniques in development of novel controlled-release systems.
Karásková, Iva ; Mravec, Filip (referee) ; Sedláček, Petr (advisor)
This diploma thesis deals with application of microencapsulation techniques in development of hydrogel controlled-release systems in which the main role is played by humic acids, biopolymer chitosan, compound fertilizer NPK and 3-indoleacetic acid. This paper continues my bachelor thesis topic about utilization of polyelectrolyte complexes. The aim of this work was to develop a literature review focusing on the microencapsulation techniques and according to its results optimize the method. Microencapsulation was performed with a commercial encapsulator BUSCHI B-395 Pro and a release of individual components into a water was measured. An amout of released substances was measured by UV-VIS method and HPLC analysis. Practical part also included testing of repeated swelling and drying. It was found that suitable composition and combination of ingredients form hydrogels for further use in agriculture.
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