1. A method for the immobilization of chitosan onto urinary cathetersAlenka Vesel, Nina Recek, Rok Zaplotnik, Albert Kurinčič, Katja Kuzmič, Lidija Fras Zemljič, 2022, original scientific article Abstract: A method for the immobilization of an antibacterial chitosan coating to polymeric urinary medical catheters is presented. The method comprises a two-step plasma-treatment procedure, followed by the deposition of chitosan from the water solution. In the first plasma step, the urinary catheter is treated with vacuum-ultraviolet radiation to break bonds in the polymer surface film and create dangling bonds, which are occupied by hydrogen atoms. In the second plasma step, polymeric catheters are treated with atomic oxygen to form oxygen-containing surface functional groups acting as binding sites for chitosan. The presence of oxygen functional groups also causes a transformation of the hydrophobic polymer surface to hydrophilic, thus enabling uniform wetting and improved adsorption of the chitosan coating. The wettability was measured by the sessile-drop method, while the surface composition and structure were measured by X-ray photoelectron spectroscopy and Fourier-transform infrared spectroscopy. Non-treated samples did not exhibit successful chitosan immobilization. The effect of plasma treatment on immobilization was explained by noncovalent interactions such as electrostatic interactions and hydrogen bonds.
Keywords: polymer, chitosan immobilization, adhesion, plasma-surface modification, biopolymers
Published in DKUM: 05.12.2024; Views: 0; Downloads: 2
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2. Novel magnetic iron oxide-dextran sulphate nanocomposites as potential anticoagulants: Investigating interactions with blood components and assessing cytotoxicityOlivija Plohl, Lidija Fras Zemljič, Boštjan Vihar, Alenka Vesel, Sašo Gyergyek, Uroš Maver, Irena Ban, Matej Bračič, 2024, original scientific article Abstract: Examining the critical role of anticoagulants in medical practice, particularly their central function in preventing abnormal blood clotting, is of the utmost importance. However, the study of interactions between blood proteins and alternative anticoagulant nano-surfaces is still understood poorly. In this study, novel approach involving direct functionalisation of magnetic iron oxide nanoparticles (MNPs) as carriers with sulphated dextran (s-dext) is presented, with the aim of evaluating the potential of magnetically-responsive MNPs@s-dext as anticoagulants. The physicochemical characterisation of the synthesised MNPs@s-dext includes crystal structure analysis, morphology study, surface and electrokinetic properties, thermogravimetric analysis and magnetic properties` evaluation, which confirms the successful preparation of the nanocomposite with sulfonate groups. The anticoagulant potential of MNPs@s-dext was investigated using a standardised activated partial thromboplastin time (APTT) test and a modified APTT test with a quartz crystal microbalance with dissipation (QCM-D) which confirmed the anticoagulant effect. Time-resolved solid-liquid interactions between the MNPs@s-dext and model blood proteins bovine serum albumin and fibrinogen were also investigated, to gain insight into their hemocompatibility, and revealed protein-repellence of MNPs@s-dext against blood proteins. The study also addressed comprehensive cytotoxicity studies of prepared nanocomposites, and provided valuable insights into potential applicability of MNPs@s-dext as a promising magnetic anticoagulant in biomedical contexts.
Keywords: dextran sulphate, magnetic nanoparticles, blood protein interactions, clot formation, anticoagulants, cytotoxicity studies
Published in DKUM: 25.07.2024; Views: 107; Downloads: 20
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3. Exploring chitosan-plant extract bilayer coatings: Advancements in active food packaging via polypropylene modificationSaša Kaloper, Olivija Plohl, Sonja Smole Možina, Alenka Vesel, Vida Šimat, Lidija Fras Zemljič, 2024, original scientific article Abstract: UV-ozone activated polypropylene (PP) food films were subjected to a novel bilayer coating process involving primary or quaternary chitosan (CH/QCH) as the first layer and natural extracts from juniper needles (Juniperus oxycedrus; JUN) or blackberry leaves (Rubus fruticosus; BBL) as the second layer. This innovative approach aims to redefine active packaging (AP) development. Through a detailed analysis by surface characterization and bioactivity assessments (i.e., antioxidant and antimicrobial functionalities), we evaluated different coating combinations. Furthermore, we investigated the stability and barrier characteristics inherent in these coatings. The confirmed deposition, coupled with a comprehensive characterization of their composition and morphology, underscored the efficacy of the coatings. Our investigation included wettability assessment via contact angle (CA) measurements, X-ray photoelectron spectroscopy (XPS), and attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR), which revealed substantial enhancements in surface concentrations of elements and functional groups of CH, QCH, JUN, and BBL. Scanning electron microscopy (SEM) unveiled the coatings' heterogeneity, while time-of-flight secondary ion mass spectrometry (ToF-SIMS) and CA profiling showed moderately compact bilayers on PP, providing active species on the hydrophilic surface, respectively. The coatings significantly reduced the oxygen permeability. Additionally, single-layer depositions of CH and QCH remained below the overall migration limit (OML). Remarkably, the coatings exhibited robust antioxidative properties due to plant extracts and exceptional antimicrobial activity against S. aureus, attributed to QCH. These findings underscore the pivotal role of film surface properties in governing bioactive characteristics and offer a promising pathway for enhancing food packaging functionality.
Keywords: chitosan, plant extracts, polypropylene, active packaging, surface characterization, bioactivity
Published in DKUM: 27.05.2024; Views: 241; Downloads: 18
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4. Loss of oxygen atoms on well-oxidized cobalt by heterogeneous surface recombinationDomen Paul, Miran Mozetič, Rok Zaplotnik, Jernej Ekar, Alenka Vesel, Gregor Primc, Denis Đonlagić, 2023, original scientific article Abstract: Calorimetry is a commonly used method in plasma characterization, but the accuracy of the method is tied to the accuracy of the recombination coefficient, which in turn depends on a number of surface effects. Surface effects also govern the kinetics in advanced methods such as atomic layer oxidation of inorganic materials and functionalization of organic materials. The flux of the reactive oxygen atoms for the controlled oxidation of such materials depends on the recombination coefficient of materials placed into the reaction chamber, which in turn depends on the surface morphology, temperature, and pressure in the processing chamber. The recombination coefficient of a well-oxidized cobalt surface was studied systematically in a range of temperatures from 300 to 800 K and pressures from 40 to 200 Pa. The coefficient increased monotonously with decreasing pressure and increasing temperature. The lowest value was about 0.05, and the highest was about 0.30. These values were measured for cobalt foils previously oxidized with oxygen plasma at the temperature of 1300 K. The oxidation caused a rich morphology with an average roughness as deduced from atomic force images of 0.9 µm. The results were compared with literature data, and the discrepancy between results reported by different authors was explained by taking into account the peculiarities of their experimental conditions.
Keywords: heterogeneous surface recombination, recombination coefficient, cobalt, cobalt oxide, temperature dependence, pressure dependence, plasma, oxygen
Published in DKUM: 26.03.2024; Views: 228; Downloads: 18
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5. Recombination of oxygen atoms on the surface of oxidized polycrystalline nickel : temperature and pressure dependencesDomen Paul, Miran Mozetič, Rok Zaplotnik, Jernej Ekar, Alenka Vesel, Gregor Primc, Denis Đonlagić, 2023, original scientific article Abstract: The recombination of neutral oxygen atoms in the ground state on the oxidized nickel samples was studied experimentally in the range of pressures where the maximum density occurs in weakly ionized low-pressure oxygen plasma, i.e. between 40 and 200 Pa. The recombination coefficient was determined in the flowing afterglow. The source of oxygen atoms was plasma sustained in a quartz tube of inner diameter 4.7 mm by a microwave discharge in the surfatron mode. The recombination coefficient was determined in the afterglow chamber, which was a Pyrex tube with an inner diameter of 36 mm. The density of oxygen atoms in the afterglow chamber was varied by adjusting the discharge power, the gas flow, the pressure, and the position of a recombinator. Such flexibility of the experimental system enabled adjustment of the temperature of the oxidized nickel samples independently from the O-atom density in its vicinity or other parameters. The density of oxygen atoms in the afterglow chamber at various system parameters was determined by the Šorli method, which is reliable, and has an accuracy of about 20%. The recombination coefficient was determined by calorimetry. The coefficient was inversely proportional to the square root of the pressure and exponentially to the sample temperature. Systematic measurements performed at various pressures and temperatures enabled empirical formula, which were explained qualitatively by recombination kinetics.
Keywords: heterogenous surface recombination, recombination coefficient, nickel, nickel oxide, temperature
Published in DKUM: 25.03.2024; Views: 243; Downloads: 21
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6. A review of recombination coefficients of neutral oxygen atoms for various materialsDomen Paul, Miran Mozetič, Rok Zaplotnik, Gregor Primc, Denis Đonlagić, Alenka Vesel, 2023, review article Abstract: Relevant data on heterogeneous surface recombination of neutral oxygen atoms available in the scientific literature are reviewed and discussed for various materials. The coefficients are determined by placing the samples either in non-equilibrium oxygen plasma or its afterglow. The experimental methods used to determine the coefficients are examined and categorized into calorimetry, actinometry, NO titration, laser-induced fluorescence, and various other methods and their combinations. Some numerical models for recombination coefficient determination are also examined. Correlations are drawn between the experimental parameters and the reported coefficients. Different materials are examined and categorized according to reported recombination coefficients into catalytic, semi-catalytic, and inert materials. Measurements from the literature of the recombination coefficients for some materials are compiled and compared, along with the possible system pressure and material surface temperature dependence of the materials’ recombination coefficient. A large scattering of results reported by different authors is discussed, and possible explanations are provided.
Keywords: heterogeneous surface recombination, recombination coefficient, surface catalicity, catalytic efficiency, atom loss coefficient, oxygen, neutral atoms, plasma
Published in DKUM: 21.03.2024; Views: 300; Downloads: 20
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7. Two-layer functional coatings of chitosan particles with embedded catechin and pomegranate extracts for potential active packagingSanja Potrč, Tjaša Kraševac Glaser, Alenka Vesel, Nataša Poklar Ulrih, Lidija Fras Zemljič, 2020, original scientific article Abstract: Two-layer functional coatings for polyethylene (PE) and polypropylene (PP) films were developed for the active packaging concept. Prior to coating, the polymer films were activated by O$_2$ and NH$_3$ plasma to increase their surface free energy and to improve the binding capacity and stability of the coatings. The first layer was prepared from a macromolecular chitosan solution, while the second (upper) layer contained chitosan particles with embedded catechin or pomegranate extract. Functionalized films were analyzed physico-chemically to elemental composition using ATR-FTIR spectroscopy and XPS. Further, oxygen permeability and wettability (Contact Angle) were examined. The antimicrobial properties were analyzed by the standard ISO 22196 method, while the antioxidative properties were determined with an ABTS assay. Functionalized films show excellent antioxidative and antimicrobial efficacy. A huge decrease in oxygen permeability was achieved in addition. Moreover, a desorption experiment was also performed, confirming that the migration profile of a compound from the surfaces was in accordance with the required overall migration limit. All these properties indicate the great potential of the developed active films/foils for end-uses in food packaging.
Keywords: plasma, chitosan, polyphenols, coating, active package
Published in DKUM: 12.07.2023; Views: 618; Downloads: 58
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8. Protein adsorption on various plasma-treated polyethylene-terephthalate substratesNina Recek, Morana Jaganjac, Metod Kolar, Lidija Milković, Miran Mozetič, Karin Stana-Kleinschek, Alenka Vesel, 2013, original scientific article Abstract: Protein adhesion and cell response to plasma-treated polymer surfaces were studied. The polymer polyethylene terephthalate (PET) was treated in either an oxygen plasma to make the surface hydrophilic, or a tetrafluoromethane CF4 plasma to make the surface hydrophobic. The plasma source was radiofrequency (RF) discharge. The adsorption of albumin and other proteins from a cell-culture medium onto these surfaces was studied using a quartz crystal microbalance (QCM), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). The cellular response to plasma-treated surfaces was studied as well using an MTT assay and scanning electron microscopy (SEM). The fastest adsorption rate was found on the hydrophilic oxygen plasma-treated sample, and the lowest was found on the pristine untreated sample. Additionally, the amount of adsorbed proteins was higher for the oxygen-plasma-treated surface, and the adsorbed layer was more viscoelastic. In addition, cell adhesion studies support this finding because the best cell adhesion was observed on oxygen-plasma-treated substrates.
Keywords: oxygen and fluorine plasma treatment, polymer surface modification, protein adsorption, cell adhesion, quartz crystal microbalance, QCM
Published in DKUM: 22.06.2017; Views: 1312; Downloads: 453
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9. Covalent binding of heparin to functionalized PET materials for improved haemocompatibilityMetod Kolar, Miran Mozetič, Karin Stana-Kleinschek, Mirjam Fröhlich, Boris Turk, Alenka Vesel, 2015, original scientific article Abstract: The hemocompatibility of vascular grafts made from poly(ethylene terephthalate) (PET) is insufficient due to the rapid adhesion and activation of blood platelets that occur upon incubation with whole blood. PET polymer was treated with NHx radicals created by passing ammonia through gaseous plasma formed by a microwave discharge, which allowed for functionalization with amino groups. X-ray photoelectron spectroscopy characterization using derivatization with 4-chlorobenzaldehyde indicated that approximately 4% of the –NH2 groups were associated with the PET surface after treatment with the gaseous radicals. The functionalized polymers were coated with an ultra-thin layer of heparin and incubated with fresh blood. The free-hemoglobin technique, which is based on the haemolysis of erythrocytes, indicated improved hemocompatibility, which was confirmed by imaging the samples using confocal optical microscopy. A significant decrease in number of adhered platelets was observed on such samples. Proliferation of both human umbilical vein endothelial cells and human microvascular endothelial cells was enhanced on treated polymers, especially after a few hours of cell seeding. Thus, the technique represents a promising substitute for wet-chemical modification of PET materials prior to coating with heparin.
Keywords: poly(ethylene terephthalate), vascular graft, biocompatibility, heparin, plasma, functionalization, haemolysis, platelet adhesion, endothelization
Published in DKUM: 21.06.2017; Views: 1344; Downloads: 351
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10. Synthesis of micro-composite beads with magnetic nano-particles embedded in porous CaCO[sub]3 matrixAlenka Vesel, Aljoša Košak, David Haložan, Kristina Eleršič, 2012, original scientific article Abstract: A method for synthesis of soft magnetic microbeads is presented. The microbeads are made from magnetic nanoparticles dispersed in CaCO3 (calcium carbonate) matrix. The composite beads are almost perfectly spherical with a diameter of few micrometers. The majority of the composite beads consists of a porous CaCO3 matrix. Magnetic nanoparticles with a size of about 10-15 nm are made of Fe2O3. They are captured inside the pores of CaCO3 matrix during its formation. CaCO3 matrix is formed by crystallization from saturated solution of sodium carbonate and calcium chloride. The composite beads are coated with a layer of functionalized polymer. The magnetic microbeads were characterized by SEM and XPS. Different functional groups were detected by XPS measurements including SO3–,NH3+,NH2,CO32– and OH groups. The results indicate that the iron oxide particles are absent on the surface and that the polymer coating serves as a good biocompatible film.
Keywords: composite, surface characterization, XPS, functionalization, Fe nanoparticles, microbeads
Published in DKUM: 23.03.2017; Views: 1335; Downloads: 116
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