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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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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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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

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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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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