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2. Preparation of Three Dimensional Structures of Polysaccharide Derivatives for Application in Regenerative Medicine : doctoral disertationAndreja Dobaj-Štiglic, 2022, doktorska disertacija Opis: Biocompatible polysaccharide scaffolds with controllable pore size, good mechanical properties, and no hazardous chemical crosslinkers are desirable for long-term tissue engineering applications. Despite decades of development of novel scaffolds, there are still many challenges to be solved regarding their production and optimization for specifically engineered tissues. Herein, we have fabricated several three-dimensional (3D) scaffolds using polysaccharide or polysaccharide-protein composite hydrogels or inks for 3D printing, featuring strong shear thinning behavior and adequate printability. The inks, composed of various combinations of chitosan, nanofibrillated cellulose, carboxymethyl cellulose, collagen, and citric acid, were 3D printed, freeze-dried, and dehydrothermally heat-treated to obtain dimensionally and mechanically stable scaffolds. The heat-assisted step induced the formation of covalent amide and ester bonds between the functional groups of chosen polysaccharides and protein collagen. Citric acid was chosen as a non-hazardous and „green” crosslinker to further tailor the mechanical properties and long-term stability of the scaffolds.
We have investigated how the complexation conditions, charge ratio, dehydrothermal treatment, and degree of crosslinking influence the scaffolds' chemical, surface, swelling, and degradation properties in the dry and hydrated states. The compressive strength, elastic modulus, dimensional stability and shape recovery of the (crosslinked) scaffolds increased significantly with balanced charge ratio, dehydrothermal treatment, and increased concentrations of citric acid crosslinker and collagen concentrations.
The prepared crosslinked scaffolds promoted (clustered) cell adhesion and showed no cytotoxic effects, as determined by cell viability assays and live/dead staining with human bone tissue-derived osteoblasts and human adipose tissue-derived mesenchymal stem cells. The water-based and non-hazardous crosslinking methods presented here can be extended to all polysaccharide- or polysaccharide-protein-based materials to develop cell-friendly scaffolds with tailored properties suitable for various tissue engineering applications. Ključne besede: chitosan, carboxymethyl cellulose, nanofibrillated cellulose, citric acid, collagen, freeze drying, 3D printing, dehydrothermal treatment Objavljeno v DKUM: 11.10.2022; Ogledov: 228; Prenosov: 47
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3. Design, Characterisation and Applications of Cellulose-Based Thin Films, Nanofibers and 3D Printed Structures : A Laboratory ManualTanja Pivec, Tamilselvan Mohan, Rupert Kargl, Manja Kurečič, Karin Stana-Kleinschek, 2021, drugo učno gradivo Opis: The introduction of the Laboratory Manual gives the theoretical bases on cellulose and its derivatives, which are used as starting polymers for the preparation of multifunctional polymers with three different advanced techniques - spin coating, electrospinning and 3D printing. In the following, each technique is presented in a separate Lab Exercise. Each exercise covers the theoretical basics on techniques for polymer processing and methods for their characterisation, with an emphasis on the application of prepared materials. The experimental sections contain all the necessary information needed to implement the exercises, while the added results provide students with the help to implement correct and successful exercises and interpret the results. Ključne besede: multifunctional polymers, polysaccharides, cellulose, electrospun, spin coating, 3D printing, nanofibers, thin films, multifunctional materials, laboratory manuals Objavljeno v DKUM: 09.03.2021; Ogledov: 555; Prenosov: 20
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4. Development of polymeric materials with rutin and polyrutin for healing of chronic leg ulcersTanja Pivec, 2018, doktorska disertacija Opis: In this work, the development of cellulose wound dressing materials with rutin (RU) and polyrutin (PR) for the healing of chronic leg ulcers is presented as a new approach of local treatment of this wound type. The flavonoid rutin is a known antioxidant substance of plant origin with wound healing promoting properties. Despite the proven beneficial properties of rutin, its potential application in wound healing is limited due to its low water solubility. This limitation can be overcome by polymerization of rutin into polyrutin. In this work an enzymatic polymerization of rutin in water without addition of organic solvents was performed to obtain a water-soluble polymer polyrutin. The chemical structure of rutin and polyrutin were investigated using UV-Vis spectroscopy, nuclear magnetic resonance spectroscopy, Fourier transform infrared spectroscopy, size-exclusion chromatography and potentiometric titrations. Biological activity related to a desired positive influence on chronic leg ulcers was investigated through the determination of the antioxidant activity, iron-chelation ability, cell viability, determination of cell proliferation and through use of the so called “scratch assay” to measure in vitro wound healing performance. Results indicate that rutin and polyrutin have a positive influence on the healing of chronic wounds. Rutin and polyrutin water dispersions at different pH and ionic strength were further characterised by means of dynamic light scattering in order to determine the size of particles and their pH dependent ζ-potential. The knowledge gained from these measurements aided the systematic interaction studies of rutin and polyrutin dispersions with cellulose-based surfaces via model and real wound healing systems. The model cellulose surfaces were thin films prepared by dissolution of trimethylsilyl cellulose in tetrahydrofuran, spin-coating of this solution on sensors of a quartz crystal microbalance (QCM-D) and subsequent regeneration of trimethylsilyl cellulose to cellulose with acid vapors. The influence of pH, salt concentration, and rutin/polyrutin concentration on the interaction with cellulose thin films was evaluated by means of a quartz crystal microbalance with dissipation. This knowledge was transferred to the application of the coatings on real wound healing systems i.e. cellulose non-wovens. The surface morphology was further characterised on model and real wound healing systems. The antioxidant activity and release kinetics were investigated for a real wound healing system, similar to the clinically used, cellulose based wound dressing materials. The main results showed that a higher solubility of polyrutin at low ionic strength contributes to the formation of continuous layers of polyrutin on cellulose surface, while the low solubility of rutin and reduced solubility of polyrutin at higher ionic strengths contribute to deposition of particles of rutin and polyrutin on the cellulose surface. The presence of particles on the surface of non-woven cellulose fibres led to a faster initial release of rutin and polyrutin. On the contrary, a continuous layer of the well soluble polyrutin contributes to a prolonged release. Namely, adsorption of the water soluble polyrutin at pH 2 without the addition of salt results in higher masses of attached polyrutin that release slower and over longer time periods. Since wound dressing materials for chronic leg ulcers often require a lower frequency of dressing change, the latter could provide an efficient therapeutic approach to their treatment. Ključne besede: Chronic wounds, Wound dressings, Cellulose, Polymerization of flavonoids, Rutin, Polyrutin Objavljeno v DKUM: 11.06.2018; Ogledov: 1315; Prenosov: 197
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5. Vpliv sinteze na velikost nanodelcevDoris Tkaučič, 2018, magistrsko delo Opis: V magistrski nalogi je predstavljena primerjava dveh metod priprave nanodelcev, znotraj dveh metod smo spreminjali parametre in spremljali vpliv sprememb na velikost nanodelcev. Nanodelci so se pripravljali iz etil celuloze po emulzijske postopku, kjer smo kot polimerne stabilizatorje uporabljali različne polisaharide, ter spreminjali njihove koncentracije. Druga uporabljena metoda je bila dializna metoda, pri kateri smo uporabili različna topila in različne koncentracije etil celuloze. Velikost delcev smo analizirali z DLS metodo in z elektronskim mikroskopom, stabilnost disperzij smo določili z določanjem zeta potenciala. Ključne besede: polisaharidi, etil celuloza, nanodelci, emulzijska metoda, dializna metoda Objavljeno v DKUM: 06.06.2018; Ogledov: 1166; Prenosov: 100
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7. Polyurethanes for medical useTanja Pivec, Majda Sfiligoj-Smole, Petra Gašparič, Karin Stana-Kleinschek, 2017, pregledni znanstveni članek Opis: Polyurethanes are synthetic copolymers containing urethane linkages in their complex chemical structure. They consist of three monomers: a diisocyanate, a polyol and a chain extender, which enables the synthesis of an endless number of polyurethanes with different physicochemical and mechanical properties. The physicochemical properties of various polyurethanes are largely dependent on the conformation of polyols, which may contain two or more different polyols, stabilisers, catalysts, liquids or solid additives and, in the case of foams, foaming agents. Depending on the structure of the polyols, i.e. the length of the chain, structure of the units (aliphatic or aromatic), ester or ether groups, or functionalisation by hydroxyl groups, polyurethanes may be flexible or rigid, and therefore suitable for various applications. In addition to the physical and chemical structure of polyurethanes, this review paper specifically addresses their use in medicine, particularly in wound dressings, tissue engineering scaffolds and drug delivery with nanoparticles and nanocapsules, and provides guidelines for the development of new biodegradable polyurethane materials. Ključne besede: segmented polyurethanes, chemical structure, reactants, medical applications Objavljeno v DKUM: 03.10.2017; Ogledov: 1354; Prenosov: 394
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8. Zeta potencial PA 6Robert Šoster, Nika Veronovski, Lidija Tušek, Karin Stana-Kleinschek, Simona Strnad, Volker Ribitsch, 2003, izvirni znanstveni članek Opis: V raziskavi smo preučevali elektrokinetične lastnosti poliamida 6 v obliki (a) folije in (b) tekstilnega filamenta ob uporabi dveh merilnih celic. Merili smo potencial zaradi pretoka in iz tega določili zeta potencial (▫$\zeta$▫ v odvisnosti od pH vrednosti medija. Meritve na posameznem materialu smo preučevali s stališča ponovljivosti. S tem namenom smo opravili meritve na 10 preskušancih istega vzorca. Določili smo osnovne statistične pokazatelje ponovljivosti za ▫$\zeta$▫ pri pH 3 in 9 ter izoelektrično tocko. Metodo smo optimirali glede na čas nabrekanja v raztopini elektrolita pred meritvijo in maso materiala v cilindrični celici. Meritve v 0,001 M KCl na obeh vrstah materiala kljub različni nadmolekulski in površinski strukturi dobro sovpadajo. Krivulje ▫$\zeta$▫=▫$\zeta$▫(pH) imajo pričakovan potek. PA 6 kaže amfoterno naravo zaradi vsebnosti amino in karboksilnih skupin. V alkalnem mediju disociirajo karboksilne skupine, kar povzroči negativen ▫$\zeta$▫ (folija: (-32,9▫$\pm$▫ 1,6) mV, filament: (-35,2▫$\pm$▫2,0) mV pri pH 9). V kislem mediju kaže PA kationski značaj zaradi disociacije amino skupin (folija: (24,5▫$\pm$▫1,7) mV, filament: (15,1▫$\pm$▫1,1) mV pri pH 3). Izoelektrična točka, kjer je ▫$\zeta$▫ enak 0, se nahaja za folijo pri pH vrednosti 4,7▫$\pm$▫0,1, za filament pa pri 4,9▫$\pm$▫ 0,1. Ključne besede: polimeri, poliamid 6, elektrokinetične lastnosti, potencial zaradi pretoka, zeta potencial, filament, folija Objavljeno v DKUM: 01.09.2017; Ogledov: 1353; Prenosov: 141
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9. Uporaba tenziometrije za zasledovanje sorpcijskih lastnosti celuloznih vlakenZdenka Peršin Fratnik, Karin Stana-Kleinschek, Tatjana Kreže, 2000, izvirni znanstveni članek Opis: Zelo pomembna lastnost tekstilnih vlaken je njihova sposobnost navzemanja tekočin - njihova sorpcijska sposobnost. Za izboljšanje reaktivnosti regeneriranih celuloznih vlaken je običajno potrebna predobdelava, kot sta pranje in beljenje. Preizkušana viskozna in modalna ter liocel vlakna so enake kemične sestave, razlikujejo se v molekulski in nadmolekulski ureditvi. Razlike v sorpcijskih lasnostih neobdelanih in predobdelanih regeneriranih celuloznih vlaken smo zasledovali z alternativno metodo - tenziometrijo ter rezultate primerjali s klasično metodo zasledovanja hidrofilnosti. Tenziometrija je analizna metoda za določevanje površinske napetosti, stičnega kota ter adsorpcije. S pomočjo Powder Contact Angle metode smo določili kapilarno hitrost preskušanih vzorcev, na osnovi tega pa izračunali stični kot med trdno (vlakno) in tekočo (voda/heptan) fazo. S postopki predobdelave se sorpcijske lasnosti regeneriranih celuloznih vlaken bistveno izboljšajo, kar ugodno vpliva na nadaljne faze plemenitenja. Največjo sorpcijsko sposobnost navzemanja vode in s tem najnižji stični kot med neobdelanimi vzorci vlaken imajo viskozna vlakna (▫$\varphi 68,3^o$▫), največji stični kot (▫$\varphi 77,1^o$▫) pa modalna vlakna. Na izboljšanje sorpcijskih lastnosti ima največji vpliv predobdelava beljenje, kjer prav tako dosežejo najnižji stični kot beljenja viskozna vlakna (▫$\varphi 57,8^o$▫). Ključne besede: tekstilna industrija, celulozna vlakna, plemenitenje, sorpcijska sposobnost, predobdelava, sorpcija, tenziometrija, regenerirana celulozna vlakna Objavljeno v DKUM: 01.09.2017; Ogledov: 987; Prenosov: 106
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10. Statistično načrtovanje postopka apretiranja viskoznih tkanin iz močno vite preje. 2.del: Apretiranje z neformaldehidnimi reagentiSeverina Iskrač, Simona Strnad, Suzana Jus, Karin Stana-Kleinschek, Majda Sfiligoj-Smole, Bojana Vončina, Mojca Poberžnik, 2004, izvirni znanstveni članek Opis: Prispevek obravnava rezultate optimiranja zamreženja tkanin iz močno vite viskozne preje z brezformaldehidnim reagentom. Proučevali smo vpliv koncentracije brezformaldehidnega reagenta za zamreženje, katalizatorja in neionogenega sredstva za mehčanje na nekatere uporabne lastnosti apretirane viskozne preje. Spremljali smo naslednje veličine: stopnjo nabrekanja viskoznih vlaken, barve razlike, pretržno silo, pretržni raztezek in kot razgubanja. Z uporabo brezformaldehidnega reagenta za zamreženje smo dosegli znižanje stopnje nabrekanja viskoznih vlaken za 51,1 do 92,4 %, povečanje kota razgubanja za 60 do 145%, zmanjšanje pretržne sile za 49% do 65% in pretržnega raztezka za 31,6 do 37,6%. Postopek zamreženja ne povzroča zaznavnik barvnih razlik in obarvanih tkanin. Ključne besede: celulozna vlakna, vrhunsko plemenitenje, brezformaldehidno zamreženje, matematično-statistične metode načrtovanja poskusov, kot razgubanja, mehanske lastnosti, barvna metrika, nabrekljivost viskoznih vlaken Objavljeno v DKUM: 31.08.2017; Ogledov: 1210; Prenosov: 95
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