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Seasonal changes in chemical profile and antioxidant activity of Padina pavonica extracts and their application in the development of bioactive chitosan/PLA bilayer film
Martina Čagalj, Lidija Fras Zemljič, Tjaša Kraševac Glaser, Eva Mežnar, Meta Sterniša, Sonja Smole Možina, María del Carmen Razola-Díaz, Vida Šimat, 2022, original scientific article

Abstract: Seaweeds are a potentially sustainable source of natural antioxidants that can be used in the food industry and possibly for the development of new sustainable packaging materials with the ability to extend the shelf-life of foods and reduce oxidation. With this in mind, the seasonal variations in the chemical composition and antioxidant activity of brown seaweed (Padina pavonica) extracts were investigated. The highest total phenolic content (TPC) and antioxidant activity (measured by ferric reducing/antioxidant power (FRAP), 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging, and oxygen radical absorbance capacity (ORAC)) were found for P. pavonica June extract. The TPC of 26.69 ± 1.86 mg gallic acid equivalent/g, FRAP of 352.82 ± 15.41 µmole Trolox equivalent (TE)/L, DPPH of 52.51 ± 2.81% inhibition, and ORAC of 76.45 ± 1.47 µmole TE/L were detected. Therefore, this extract was chosen for the development of bioactive PLA bilayer film, along with chitosan. Primary or quaternary chitosan was used as the first layer on polylactic acid (PLA) films. A suspension of chitosan particles with entrapped P. pavonica extract was used as the second layer. X-ray photoelectron spectroscopy confirmed the presence of layers on the material surface. The highest recorded antioxidant activity of the newly developed films was 63.82% inhibition. The developed functional films exhibited antifogging and antioxidant properties, showing the potential for application in the food industry.
Keywords: functional PLA films, seaweed and chitosan bilayer, sustainable natural antioxidants, microwave-assisted extraction
Published in DKUM: 23.08.2023; Views: 115; Downloads: 10
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Green techniques for preparation of red beetroot extracts with enhanced biological potential
Dragana Borjan, Vanja Šeregelj, Darija Cör Andrejč, Lato Pezo, Vesna Tumbas Šaponjac, Željko Knez, Jelena J. Vulić, Maša Knez Marevci, 2022, original scientific article

Abstract: Red beetroot is well known for its high proportion of betalains, with great potential as functional food ingredients due to their health-promoting properties. The objective of this study was to investigate the influence of processing techniques such as Soxhlet, cold, ultrasound and supercritical fluid extraction on the betalains content and its antioxidant, anti-inflammatory and antihyperglycemic activities. Whilst Soxhlet extraction with water has provided the highest yield, the highest content of total phenolics was found in an extract prepared using Soxhlet extraction with 50% ethanol. Amongst eight phenolic compounds detected in the extracts, protocatechuic acid was the most abundant. The concentrations of total phenolics ranged from 12.09 mg/g (ultrasound extraction with 30% methanol) to 18.60 mg/g (Soxhlet extraction with 50% ethanol). The highest anti-inflammatory activity was observed for cold extraction with 50% methanol extract. The high radical scavenging activity of supercritical fluid extracts could be a consequence of nonphenolic compounds. The chemometrics approach was further used to analyse the results to find the “greenest” method for further possible application in the processing of beetroot in the food and/or pharmaceutical industry. According to the standard score, the best extraction method was determined to be Soxhlet extraction with 50% ethanol.
Keywords: red beetroot, supercritical fluid extraction, antioxidant activity, anti-inflammatory activity, antihyperglycemic activity, chemometric approach
Published in DKUM: 18.08.2023; Views: 153; Downloads: 11
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The effect of drying methods and extraction techniques on oleuropein content in olive leaves
Darija Cör Andrejč, Bojan Butinar, Željko Knez, Kaja Tomažič, Maša Knez Marevci, 2022, original scientific article

Abstract: Increased demand for olive oil has caused higher quantities of byproducts in olive processing, such as olive leaves, olive skins, and vegetation water. It is well known that olive leaves contain several phenolic compounds, including secoiridoids. Oleuropein is the major secoiridoid in olive leaves. Oleuropein has been found to exhibit antioxidative, antimicrobial, antiviral, and antiatherogenic activities. We studied the effect of extraction techniques and drying methods on oleuropein content in olive leaves of Istrska belica and Lecino cultivar. Three different procedures of drying were used: at room temperature, at 105 °C, and freeze drying. Ethanol-modified supercritical extraction with carbon dioxide, conventional methanol extraction, and ultrasonic extraction with deep eutectic solvent were performed. Antioxidant activity was determined, as well as methanolic and supercritical extracts. The presence of olive polyphenols was confirmed by the HPLC method.
Keywords: olive leaves, drying, different extraction techniques, oleuropein
Published in DKUM: 10.08.2023; Views: 113; Downloads: 11
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Sustainable processing of materials using supercritical fluids : doktorska disertacija
Dragana Borjan, 2022, doctoral dissertation

Abstract: Supercritical fluids (SCFs) are powerful solvents with many unique properties. They have great potential for many processes, from extraction to chemical reactions and recycling. Accordingly, phase equilibrium data and thermodynamic and transport properties measurements in systems with a supercritical phase, as well as reliable and versatile mathematical models of the phase equilibrium thermodynamics, are needed for the process design and economic feasibility studies. The dissertation focuses on the benefits of supercritical fluid technology and consists of three main sections. The first section includes studies of the phase equilibria of the binary gas-alcohol and gas-urea derivatives. The influence of pressure and temperature on the system behaviour (solubility, viscosity, density, interfacial tension, melting point curve) was investigated. Most of the experiments were carried out with a high-pressure optical view cell, with minor modifications of the apparatus and measurement principle to determine mentioned thermodynamic and transport properties. The second part of the dissertation deals with the recovery of extracts from natural materials. Special interest is oriented towards supercritical fluid extracts, characterised by strong biological activities, especially antimicrobial and antioxidant properties. Supercritical fluid extraction has been performed on a semi-continuous apparatus (at pressures of 150 bar and 250 bar and temperatures of 313.15 K and 333.15 K for oregano extraction; and at pressures of 100 bar and 300 bar and temperatures of 313.15 K and 333.15 K for red beetroot extraction) and various methods such as the microdilution method and the DPPH method were used to determine antimicrobial and antioxidant activity. In the third part, an overview of different methods for recycling carbon fibre reinforced composites is given, including chemical recycling with supercritical fluids. This field has not been well explored, and the approach is relatively new but very interesting from a sustainable point of view. For an economically feasible process design, the thermodynamic and mass transfer data have to be determined. The principles of the future lab- and pilot-scale operations demand these supporting data be known. The results obtained in the frame of this study represent the high added value in the scientific field. They are essential to design and modify processes that yield products that cannot be achieved with conventional production processes.
Keywords: supercritical fluids, alcohols, urea, phase equilibria, viscosity, density, interfacial tension, modified capillary method, isolation methods, supercritical fluid extraction, pharmacological activity, carbon fiber reinforced composites, recycling techniques
Published in DKUM: 11.10.2022; Views: 581; Downloads: 111
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Optimizacija postopka ekstrakcije učinkovin iz arnike arnica montana in formulacija produktov : master's thesis
Álvaro Pequeno Alonso, 2022, master's thesis

Abstract: Arnica Montana je obetaven vir bioaktivnih spojin, predvsem fenolov, ki zaradi svoje antioksidativne aktivnosti izkazujejo koristi za zdravje ljudi. Da bi dosegli stopnjo farmacevtske uporabe, je treba cvetove Arnice Montana predelati v izdelek, ki je primeren za preživetje. V ta namen so bile izvedene različne ekstrakcijske tehnike z različnimi topili: hladna maceracija, ultrazvok, Soxhlet in superkritični CO2; uporabljena topila so bila etanol, metanol in mešanica etanola in vode 95:5 (v:v). Analiza, ki je vključevala ultravijolično/vidno spektrometrijo, je bila opravljena za merjenje antioksidativne aktivnosti in celotne vsebnosti fenolov v ekstraktih. Končno je bil organogel oblikovan z uporabo izvlečka, olja konoplje in voska riževih otrobov ter testiran glede njegove stabilnosti. V okviru tega dela je bil prvič formuliran organogel z visoko stabilnostjo, saj do sedaj v znanstveni literaturi ni bilo podatkov o tovrstni formulaciji. Za določitev njegovih reoloških lastnosti in topnosti v različnih topilih pri različnih temperaturnih pogojih bodo potrebne dodatne študije.
Keywords: Arnica Montana, organogels, solvent extraction, phenolic compounds, isolation, formulation
Published in DKUM: 13.07.2022; Views: 371; Downloads: 31
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AI for optimizing analog RF parameters on NFC frontends : magistrsko delo
Matej Žnidarič, 2022, master's thesis

Abstract: In this Master’s thesis, we study in detail NFC technology, NFC standardization, Artificial intelligence and GUI topics.Our goal is to optimize the measurement process of the FeliCa listener phase window in order to define the best analog parameters for the NFC IC. Namely, by combining machine learning and test automation, we want to achieve a faster validation time of the NFC IC under test. Firstly, we introduce the main topics related to NFC and present the thesis alongside specific goals. Next, we present the NFC technology on a fewuse cases. We also cover international standards, emphasizing sections that directly affect our validation and, therefore, the understanding of our solution. The NFC coverage is described alongside data representation used to interpret data used in proprietary software. Artificial intelligence is integrated into this software for multidimensional data interpolation task. We also cover the basics of deep neural networks and the most common architectures used in the DL field. The neural network training process is also covered to understand how we can optimize neural network global minimum convergence. In the last part of the thesis, we also explain how proprietary software tool actually works and how it can outperform previous processes. In the end, specific solutions related to the tool are described in more detail to understand our software development decisions better. Finally, we present measurement results and evaluate our goals.
Keywords: NFC wireless communication, artificial intelligence, test coverage, FeliCa, graphical user interface, analog parameter extraction
Published in DKUM: 08.06.2022; Views: 842; Downloads: 0

Hydrothermal processes for conversion of lignocellulosic biomass to value-added compounds : doctoral disertation
Tanja Milovanović, 2020, doctoral dissertation

Abstract: In this doctorial dissertation subcritical water processes of lignocellulosic biomass to obtain value-added compounds are studied. The doctorial dissertation is divided into four main parts. In the first and second part of dissertation, model compounds (standards of cellulose and sugars and chestnut tannins) were primarly used in order to better understand processes of real biomass material. The degradation of cellulose and different sugars was performed in batch reactor with subcritical water. The different reaction temperatures and times were used. The main phases, such as water-soluble fraction, acetone-soluble fraction and solid residue were separated and analysed. The analysis of water-soluble phase was done by HPLC equipped with UV and RI detector, while acetone-soluble phase of cellulose was analysed by GC-MS. Total sugar content was determined by the phenol-sulphuric acid colorimetric method. The properties of char, obtained using cellulose as a treated material, such as: specific surface area, pore volume and pore diameter were determined by gas adsorption method. A water-soluble phase mainly consists of sugar monomers and monomer degradation products such as 5-hydroxymethylfurfural (5-HMF), furfural, erythrose, sorbitol, 1,6-anhydroglucose, glycolaldehyde, glycerlaldehyde, 1,3-dihydroxyacetone, pyruvaldehyde, formic, levulinic, lactic, oxalic and succinic acids, while acetone-soluble phase, referred to also as bio-oil, consists of furans, phenols, carboxylic acids, aldehydes, ketones and high molecular compounds. The reaction mechanism of cellulose and sugars in subcritical water has been proposed based on the obtained results. Furthermore, the results from cellulose and sugar hydrothermal degradation were utilized in further work to determine which industrially interesting products could be obtained by hydrothermal processing of paper waste in subcritical water. The optimum conditions ( temperature and reaction time), which gave us the highest yield of base chemicals (furfural, 5-HMF, levulinic acid) were determined. Sweet chestnut (Castanea Sativa) bark contains high level of tannins and various phenolic compounds which can be utilized in pharmaceutical, cosmetic, nutritional and medical purposes. The sweet chestnut tannins extract and sweet chestnut bark were used as materials highly rich in bioactive compounds for subcritical water processes which are presented in the second part of doctorial dissertation, respectively. The spectrophotometric methods were used to determine total tannins, phenols and carbohydrates content and antioxidant activity. The identified compounds were ellagic and gallic acid, ellagitannins (vescalagin, castalagin, 1-o-galloyl castalagin, vescalin and castalin), sugars (maltose, glucose, fructose and arabinose) and sugar derivatives (5-HMF, furfural and levulinic acid). The results obtained from hydrothermal hydrolysis were compared to results from acid hydrolysis. Finally, the optimization of reaction parameters of subcritical water processes has been done aiming to obtain the product highly rich in ellagic acid. Subcritical water extraction of horse chestnut (Aesculus hippocastanum) parts such as seeds, seed shell, bark and leaves was described in the third chapter of dissertation. The detected compounds in extracts, such as escins, esculin, fraxin, phenolic compounds (chlorogenic, neochlorogenic and gallic acids) and furfurals (5-hydroxymethyfurfural, furfural, and methylfufrual) are quantified using HPLC. The last part of dissertation proposes extraction of cocoa shell using green technologies (supercritical CO2 and subcritical water extraction) and also conventional methods (Soxhlet extraction with hexane and extraction with 50 % acetone) to obtain bioactive compounds in order to compare the results. The detected compouns were methylxanthines, phenolic compounds, sugars, fatty acids.
Keywords: Subcritical water, biomass, biowaste, extraction, hydrothermal degradation, hydrolysis, bioactive compounds.
Published in DKUM: 16.10.2020; Views: 1324; Downloads: 150
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Development of analytical methods for simultaneous identification and determination of phenolic compounds
Milena Ivanović, 2018, doctoral dissertation

Abstract: The objective of this doctoral dissertation was to develop different analytical approaches for the extraction, separation, identification and quantitative determination of various phenolic compounds from different plants and their products. This dissertation is divided into the following four major segments, which, to some extent, can stand alone, but when it comes to the research, they are mutually very related: - Segment 1: Short-term (up to 24 h) and long-term (up to 1 month) stability studies of trans-caffeic acid (trans-CA) and trans-ferulic acid (trans-FA) dissolved in two organic solvents (methanol and tetrahydrofuran) and exposed to a range of storage conditions (temperature, organic solvents used, influence of daylight and UV irradiation) were performed for the first time. Gas chromatography with mass spectrometry (GC-MS) was used to study the degradation of the samples and structural identification of the degradation products. - Segment 2: The research within this segment focused on the optimization of a simple, fast and quantitative extraction method for the isolation of phenolic acids (PAs) from Slovenian red wine samples. Different extraction techniques were tested, and solid phase extraction (SPE) using HLB cartridges was selected as the optimal technique. For the identification and quantification of extracted analytes, the GC-MS method was optimized and validated. Different statistical and chemometrical tools were applied, and the wines were classified according to the Slovenian wine-growing regions and vine varieties. - Segment 3: The main goal within this research segment was the development of an ultrasound-assisted extraction (UAE) method for the isolation of different polyphenol classes from coriander fruits. Additionally, for the isolation of total PAs (free and bound), two analytical steps were applied: UAE alkaline hydrolysis and clean-up using SPE HLB cartridges. The response surface methodology (RSM) combined with a Box-Behnken experimental design (BBD) were used for the optimization of the alkaline hydrolysis and for increasing the extraction yields of the PAs. In this way, most influencing factors (temperature, sonication time and NaOH concentration) were studied as independent variables. Extracted PAs were determined using the previously optimized GC-MS method. - Segment 4: The main goal of this segment of the dissertation was to show the application of deep eutectic solvents (DESs) as a ‘green’ alternative to the conventional organic solvents for the isolation of phenolic compounds from plants such as Aronia melanocarpa (dried chokeberry) and Olea europaea (olive leaves). Different extraction techniques and instrumental methods were applied for the determination of phenolic profiles. Phenols from chokeberries were obtained through UAE. Furthermore, for the simultaneous identification and quantitative determination of 21 different phenolic compounds from Aronia melanocarpa, the HPLC-UV method was optimized and validated. On the other hand, microwave-assisted extraction (MAE) was used to improve the extraction yields of phenolic compounds from olive leave samples, which were subsequently determined by using validated HPLC-DAD-ESI-TOF-MS method.
Keywords: phenolic compounds, phenolic acids, extraction, GC-MS, HPLC, method optimization, deep eutectic solvents, plant material
Published in DKUM: 11.04.2018; Views: 1960; Downloads: 165
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Applying automated model extraction for simulation and verification of real-life SDL specification with spin
Boštjan Vlaovič, Aleksander Vreže, Zmago Brezočnik, 2017, original scientific article

Abstract: Formally defined Specification and Description Language (SDL) is used for the design and specification of complex safety-critical systems. Each change in the specification of the product should be immediately checked formally against the requirements’ specification. This paper presents semi-automated system abstraction, automated model extraction, simulation, and formal verification of real-life complex SDL specification. Sound algorithms implemented in our sdl2pml automated model extraction tool preserve all properties of the SDL system. Sdl2pml includes our model of discrete time, abstraction, and support for all relevant SDL functionality and constructs such as dynamic process creation, rational data types, and communication with more than one process instance. To the best of our knowledge, most of them are not supported by any other known approach. We use our SpinRCP tool for simulation and formal verification of the extracted model with the Spin model checker. We demonstrate the applicability of our approach on ISDN User adaptation protocol from SI3000 Softswitch. The extracted Promela model is the largest one ever processed by Spin. We have shown that Spin simulation and model checking can be applied successfully to such huge models.
Keywords: formal specifications, automated extraction, formal languages, simulation, formal verification, model cheking, SDL, Promela, SpinRCP, Sdl2pml
Published in DKUM: 03.08.2017; Views: 1188; Downloads: 413
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Extraction and separation of active compounds by supercritical fluids extraction and preparative supercritical chromatography
Alejandro Bartolome Ortega, 2017, doctoral dissertation

Abstract: This doctoral dissertation is focused on the benefits of supercritical fluids technology in several industry processes. Although, supercritical CO2 is currently the most employed supercritical fluid at laboratory scale, its presence in the industry field is still limited, due to the necessity of high investment costs. Despite that fact, operations with supercritical CO2 are cheap, environmentally friendly and simple, which make it an excellent alternative to organic compounds. Extraction and separation of highly pure active compounds, such as xanthohumol or beta-sitosterol, are demanded for pharmaceutical or food industries, which create an excellent opportunity for supercritical CO2 operations, since they are solvent free. This manuscript is divided into three different parts. In the first part, conventional extraction processes and supercritical fluid process are theoretically compared and supercritical fluid extraction from saw palmetto berries is presented. In the second part, conventional chromatographic techniques and supercritical fluid chromatography are theoretically compared and separation of xanthohumol from hop extracts by supercritical fluid chromatography is presented. In the last part, different encapsulation and emulsification processes are listed and defined. These processes are very important for food and pharmaceutical companies, since several active compounds are not water soluble which create the necessity of different formulations in order to be solved in an appropriate media. Regarding the experimental part, extractions from saw palmetto berries were performed at various pressures and temperatures, which were higher than the ones that were applied in previous studies, in order to estimate and calculate different parameters (solubility, extraction kinetic curves, composition,…), and to compare different studies. Separation of xanthohumol was carried out in a homemade supercritical chromatography, which manageable variables were temperature, pressure, mass flow-rate, modifier, and stationary phase. The results were compared with those ones which were obtained using conventional techniques, in order to prove the suitability and the improvement of this technique against others tecniques.
Keywords: supercritical CO2, supercritical fluid extraction, supercritical fluid chromatography, xanthohumol, saw palmetto berries, Beta-Sitosterol, encapsulation
Published in DKUM: 13.07.2017; Views: 1933; Downloads: 241
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