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Development of pH Responsive Polysaccharide Based Wound Dressings : doctoral disertation
Beste Elveren, 2023, doctoral dissertation

Abstract: In the scope of the Doctoral Dissertation, a polysaccharide based stimuli-responsive smart material with controlled drug release was developed by using electrospinning technique, which allowed to form stimuli-responsive nanofibers with rapid visual detection of pH change in the wound bed along with anti-inflammatory activity. Incorporation of halochromic dyes into electrospun nanofibers has been an intriguing area for wound healing applications. Furthermore, it is known that the pH value within the wound milieu directly and indirectly influences all biochemical reactions taking place in the process of wound healing. It has been proven that the surface pH of a wound plays an important role in wound healing as it helps control infection and increases the antimicrobial activity, oxygen release, angiogenesis, protease activity, and bacterial toxicity. Therefore, visual pH monitoring without the need of removing the wound dressing was one of the aims of the Doctoral Dissertation. Produced stimuli-responsive wound dressings were characterized according to their morphological and chemical properties using well-known techniques such as, rheometry, conductivity, Scanning Electron Microscopy (SEM),CIE Lab, Thermogravimetric Analysis (TGA), UV/VIS Spectrophotometry, and Attenuated Total Reflection Infra-Red Spectroscopy (ATR-IR). Responsiveness of the nanofibers were achieved by integration of different halochromic dyes [bromocresol green (BCG), bromothymol blue (BTB) and thymol blue (TB)] to obtain a range of pH values. To tackle the problem of leaching of the dyes, a complexing agent; poly-diallyldimethylammonium chloride (PDADMAC) was integrated and an analysis on the formation of complexation was performed by using pH-potentiometric titration and Quartz Crystal Microbalance with Dissipation (QCM-D) and Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) techniques. Additionally, release tests were performed to prove that the leaching of the halochromic dyes is reduced significantly up to 97%. Furthermore, the responsiveness of the nanofibers was investigated by exposing the nanofibers to different buffer solutions with pH values 4, 7 and 10. The color change of the nanofibers were analyzed using the CIE Lab system while a visual color shift was observed according to their characteristics. Lastly, diclofenac (DFC), an anti-inflammatory drug molecule was integrated to the system and drug release studies were performed by using Franz diffusion cells. A controlled release of the drug molecule (DFC) to the wound bed is achieved and quantitative evaluations were done. Consequently, the drug release from the smart wound dressings were identified to have two separate profiles during the release. The mathematical models that were identified to fit to the kinetics are, first-order, Korsmeyer-Peppas, and Higuchi release model, confirming the controlled drug release.
Keywords: stimuli-responsive, polysaccharides, wound dressings, halochromism, controlled drug release, smart materials
Published in DKUM: 06.10.2023; Views: 375; Downloads: 33
.pdf Full text (8,48 MB)

Antioxidant, antibacterial, antitumor, antifungal, antiviral, anti-inflammatory, and nevro-protective activity of Ganoderma lucidum : an overview
Darija Cör Andrejč, Željko Knez, Maša Knez Marevci, 2022, review article

Abstract: Ganoderma lucidum is a very medicinal mushroom that has been utilized in Oriental medicine for many years. It has a wide range of pharmacological and therapeutic properties, and has been used for many years as a health promoter. It contains various biologically active compounds that improve the immune system and have antioxidant, antitumor, anti-inflammatory, antifungal, and antimicrobial properties. Active compounds include triterpenoids and polysaccharides, as well as proteins, lipids, phenolics, sterols, etc. In the following review, we summarize briefly their biological activities, such as antioxidant, anti-bacterial, anti-fungal, antitumor, anti-viral, and anti-inflammatory activity. Although Ganoderma has a number of medicinal effects that have been confirmed by the in vitro and in vivo studies summarised in this review, there are some limitations. Clinical trials face mainly a lack of pure constituents. Accurate identification of the compounds obtained is also problematic. In addition, most of the included studies were small, and there were concerns about the methodological quality of each study. Studies have shown that Ganoderma has valuable potential for the prevention and treatment of cancer. In any case, G. lucidum cannot be used as first-line therapy for cancer.
Keywords: Ganoderma lucidum, bioactive function, active compounds, polysaccharides, triterpenoids
Published in DKUM: 16.08.2023; Views: 285; Downloads: 30
.pdf Full text (1,26 MB)
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Fabrication of polysaccharide-based halochromic nanofibers via needle-less electrospinning and their characterization: a study of the leaching effect
Beste Elveren, Silvo Hribernik, Manja Kurečič, 2022, original scientific article

Abstract: Responsive materials, i.e., smart materials, have the ability to change their physical or chemical properties upon certain external signals. The development of nanofibrous halochromic materials, specifically combining the pH-sensitive functionality and unique nanofiber properties, could yield interesting new applications, especially when the common problem of dye leaching is successfully tackled. Therefore, in this article, we studied the fabrication process of polysaccharide-based halochromic nanofibrous materials by using a combination of various halochromic dyes (bromothymol blue, bromocresol green, and thymol blue) and cellulose acetate in a spinning solution using a one-pot strategy. The inhibition of leaching was addressed by using a complexing agent: poly-diallyl-dimethylammonium chloride (PDADMAC). The preparation of hybrid spinning solutions, their characterization, and ability to form continuous nanofibers were studied using a high production needle-less electrospinning system. The produced hybrid solutions and nanofibers were characterized, in terms of their rheological properties, chemical structure, morphology, and functionality. Fabricated nanofibrous halochromic structures show a clear color change upon exposure to different pH values, as well as the reduced leaching of dyes, upon the addition of a complexing agent. The leaching decreased by 61% in the case of bromocresol green, while, in the case of bromothymol blue and thymol blue, the leaching was reduced by 95 and 99%, respectively.
Keywords: halochromism, responsive polymers, polysaccharides, electrospinning
Published in DKUM: 31.07.2023; Views: 387; Downloads: 44
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Design, Characterisation and Applications of Cellulose-Based Thin Films, Nanofibers and 3D Printed Structures : A Laboratory Manual
Tanja Pivec, Tamilselvan Mohan, Rupert Kargl, Manja Kurečič, Karin Stana-Kleinschek, 2021, other educational material

Abstract: 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.
Keywords: multifunctional polymers, polysaccharides, cellulose, electrospun, spin coating, 3D printing, nanofibers, thin films, multifunctional materials, laboratory manuals
Published in DKUM: 09.03.2021; Views: 917; Downloads: 24
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Jorge Rodríguez Antolín, 2020, undergraduate thesis

Abstract: The following work examines the possibility of impregnating chosen model drug into bioaerogels to obtain final formulation with added value. The drug used in this study was esomeprazole, used to treat acid-related diseases. In the first part of the work, bioaerogels were prepared. Polysaccharide aerogels are lightweight biocompatible and biodegradable materials, suitable for applications in pharmaceutical industry. For this purpose, three different cores were prepared: pectin, alginate and their mixture, followed by coating with chitosan layer. The production of the bioaerogels follows a sol-gel synthesis and supercritical drying technique. All samples were characterised, and optimisation was performed based on examined properties. Aerogels having a pectin core and chitosan coating showed the highest surface area and the highest adsorption capacity. In the second part, the impregnation of esomeprazole was performed using two different methods: supercritical impregnation and diffusion via sol-gel synthesis. For supercritical impregnation, supercritical carbon dioxide was used as a solvent for impregnation of the drug. In the diffusion method, the model drug was added during sol-gel synthesis using ethanol as solvent. Finally, complete characterisation of prepared formulation followed by drug release studies was performed. The study showed successful impregnation of esomeprazole using either carbon dioxide or ethanol as a solvent. Bioaerogels proved to be promising as carriers for achieving the optimal release of the chosen drug.
Keywords: Bioaerogels, polysaccharides, supercritical impregnation, diffusion method, esomeprazole
Published in DKUM: 09.07.2020; Views: 889; Downloads: 54
.pdf Full text (1,28 MB)

Formation, characterization and application of polysaccharide aerogels
Gabrijela Horvat, 2018, doctoral dissertation

Abstract: The aim of this PhD dissertation was to describe and analyze the preparation and characterization of polysaccharide aerogels and their future pharmaceutical and medical application. For the research, we used four types of polysaccharides: pectin, alginate, xanthan and guar. We used two types of pectin, high-methoxyl and low-methoxyl pectin, because of their different gelation mechanisms. The first part of the dissertation describes the preparation and characterization of pure polysaccharide aerogels. First, we prepared pectin spherical aerogels, cross-linked with three different ions, and we investigated their final properties. Later, we developed a new method for the preparation of alginate, pectin, xanthan and guar aerogels. We used only ethanol and no other cross-linkers. Ethanol was removed in the later processes of supercritical drying, and the remaining final material was thus only porous polysaccharide. By this method, we were able to prepare pure xanthan and guar aerogels. Prior to this study, xanthan and guar aerogels were prepared only as composites. Pectin aerogels prepared by the new method have amazing properties. On the other hand, alginate aerogels show poor characteristics, and thus the methods need to be optimised. We tried different alginate viscosities, different alcohols (methanol, ethanol, 1-propanol and 1-butanol), and we investigated longer (24h) and shorter (1h) gel setting times. The second part of this dissertation describes the pharmaceutical and medical applications of prepared aerogels. The release of diclofenac sodium from spherical pectin aerogels was investigated in vitro. Calcium cross-linked aerogels were not able to retain the drug, and its release was immediate. In order to achieve controlled release of diclofenac sodium, zinc ions had to be used as cross-linkers. Later, a low water-soluble drug, nifedipine, was used as a model drug for the monolithic aerogels prepared by the new method. The release of nifedipine from pectin and alginate aerogels was highly increased, compared to the crystalline drug. This result is promising for future evaluation of these materials for increasing the bioavailability of poorly water-soluble drugs. Nifedipine release from xanthan and guar aerogels was prolonged up to two weeks. This result reveals a new perspective on such materials for their potential use in medicine as implants and local drug delivery. According to these results, we then developed a new coating material for medical-grade stainless steel from xanthan and pectin. An aerogel coating was loaded with diclofenac sodium and indomethacin, and their release profiles were investigated in vitro. Electrochemical analysis and cell tests proved the safety of such materials for use in medicine. Using aerogel coatings, the drug can be introduced locally into the body; therefore, the need for intravenous, post-operational treatment is greatly reduced.
Keywords: polysaccharides, aerogels, supercritical drying, drug carriers
Published in DKUM: 09.04.2018; Views: 2047; Downloads: 282
.pdf Full text (5,84 MB)

Surface modification of silicone with polysaccharides for the development of antimicrobial urethral catheters
Matej Bračič, 2016, doctoral dissertation

Abstract: In this work, alternative polysaccharide-based coatings were used to improve the antimicrobial and antifouling properties of silicone surfaces used for urethral catheters. The introduction of a catheter in the urethra is commonly connected with a high risk of microbial infections which often result in long-term health damage. Polysaccharide-based coatings like chitosan, carboxymethyl chitosan, and a synergistic formulation between hyaluronic acid and a natural lysine-based surfactant, were used to treat silicone surfaces to overcome the infection problems as an alternative to conventional approaches, which include the administration of antibiotics or coatings with metal ions. The polysaccharide-based macromolecular solutions and dispersions were firstly characterised by means of pH-titrations, dynamic light scattering and scanning electron microscopy in order to determine the size of particles in dispersions and their pH dependant charging behaviour. The knowledge gained from this was used to thoroughly study the interactions of the polysaccharide-based solutions and dispersions with the model silicone surfaces. The model surfaces were ultra-thin films prepared by dissolution of silicone in toluene and subsequent spin-coating on quartz crystals. The influence of pH, salt concentration, and various surface activation processes on the adsorption behaviour was evaluated by means of a very precise quartz crystal microbalance with dissipation. This knowledge was transferred to the application of the coatings on real systems i.e. casted silicone sheets and silicone tubes. The surface morphology, surface chemistry, as well as the mechanical and chemical stability of the coatings were further characterised on both model and real systems. For this purpose different microscopy and spectroscopy methods, pH-potentiometric titrations and methods for evaluation of mechanical properties were used. Finally the antimicrobial and antifouling properties were evaluated. The antimicrobial properties were tested against gram-positive and gram-negative bacteria as well as fungi, which are commonly found in infected urine, while the antifouling properties were tested by measuring the adhesion of bovine serum albumin, fibrinogen, and lysozyme biomolecules onto functionalised model films using the quartz crystal microbalance. The results showed that homogeneous and stable coatings can be achieved by adsorption from dispersions of the polysaccharide-based nanoparticles of 200-300 nm in size, which are formed by precipitation; i.e. careful pH adjustments of chitosan to pH = 6.5, carboxymethyl chitosan to pH = 7, and by mixing the hyaluronic acid and natural lysine-based surfactant solutions at concentrations of 2.5 x 10-4 mol/L and 1.25 x 10- 3 mol/L for the hyaluronic acid and 5.0 x 10-4 mol/L and 1.2 x 10-3 mol/L for the surfactant, respectively . The mass of the coatings on model silicone films can be increased by a 3-step adsorption, which directly influences the antimicrobial properties of the coatings that are improved with increasing coating mass, reaching values of up to 90 % in reduction of microorganism growth. It was also shown that the hyaluronic acid-natural surfactant formulation is superior to the chitosan coatings. The same conclusions were drawn from the antifouling evaluation where the zwitterionic nature of the formulation between natural based lysine surfactant and HA successfully suppressed the adhesion of biomolecules on silicone surfaces, while the chitosan coatings only moderately prevented the adhesion of proteins. One can conclude that the polysaccharide-based coatings can be successfully introduced to silicone surfaces from dispersion and as such successfully prevent biomolecule adhesion and reduce the growth of pathogen microorganisms which can be found in the urine during urethral infections.
Keywords: Urethral catheters, Antimicrobial coatings, Silicone, Polysaccharides, Natural surfactants
Published in DKUM: 24.10.2016; Views: 2209; Downloads: 234
.pdf Full text (5,86 MB)

Future Perspectives in Polysaccharide Research : book of abstracts
2016, other monographs and other completed works

Keywords: polysaccharides, polysaccharide based materials
Published in DKUM: 19.09.2016; Views: 1523; Downloads: 74
.pdf Full text (1,90 MB)

Rheological studies of concentrated guar gum
Marija Oblonšek, Sonja Šostar-Turk, Romano Lapasin, 2003, original scientific article

Abstract: Polymers and surfactants are essential ingredients of the printing paste. Polysaccharides are used commercially to thicken, suspend or stabilise aqueoussystems. Also they are used to produce gels and to act as flocculates, binders, lubricants, to serve as modifiers of film properties, and have a function as adjusters of rheological parameters. Surfactants, on the other hand, perform numerous functions acting as dispersants, wetting agents, emulsifiers and antifoaming agents. The rheological properties of polysaccharide thickeners (guar gums with different substitution levels and different producers) at different concentrations and temperatures and, second,the effects produced by the addition of nonionic surfactants (polyoxyethylene stearyl alcohols with different numbers of EO groups) have been studied under linear and nonlinear shear conditions. Experimental data have been correlated with the different modelsČ flow curves with the Cross, Carreau and Meter-Bird model, and mechanical spectra with the generalized Maxwell model and Friedrich-Braun model. The surface tensions of aqueous systems containing polysaccharide andžor surfactants have been determined overextended concentration ranges in order to detect the CMC conditions and toprovide a better understanding about the polysaccharide-surfactant interactions.
Keywords: textile printing, printing pastes, polysaccharides, thickeners, rheology, viscoelasticity, surfactants, guar gum
Published in DKUM: 01.06.2012; Views: 2501; Downloads: 88
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