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1.
Hydrothermal processes for conversion of lignocellulosic biomass to value-added compounds
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: 16.10.2020; Views: 319; Downloads: 55
.pdf Full text (6,32 MB)

2.
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: 11.04.2018; Views: 1030; Downloads: 96
.pdf Full text (5,10 MB)

3.
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: 03.08.2017; Views: 713; Downloads: 318
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4.
Polyphenols: extraction methods, antioxidative action, bioavailability and anticarcinogenic effects
Eva Brglez Mojzer, Maša Knez Hrnčič, Mojca Škerget, Željko Knez, Urban Bren, 2016, original scientific article

Abstract: Being secondary plant metabolites, polyphenols represent a large and diverse group of substances abundantly present in a majority of fruits, herbs and vegetables. The current contribution is focused on their bioavailability, antioxidative and anticarcinogenic properties. An overview of extraction methods is also given, with supercritical fluid extraction highlighted as a promising eco-friendly alternative providing exceptional separation and protection from degradation of unstable polyphenols. The protective role of polyphenols against reactive oxygen and nitrogen species, UV light, plant pathogens, parasites and predators results in several beneficial biological activities giving rise to prophylaxis or possibly even to a cure for several prevailing human diseases, especially various cancer types. Omnipresence, specificity of the response and the absence of or low toxicity are crucial advantages of polyphenols as anticancer agents. The main problem represents their low bioavailability and rapid metabolism. One of the promising solutions lies in nanoformulation of polyphenols that prevents their degradation and thus enables significantly higher concentrations to reach the target cells. Another, more practiced, solution is the use of mixtures of various polyphenols that bring synergistic effects, resulting in lowering of the required therapeutic dose and in multitargeted action. The combination of polyphenols with existing drugs and therapies also shows promising results and significantly reduces their toxicity.
Keywords: polyphenols, extraction, antioxidants, bioavailability, synergistic effects
Published: 22.06.2017; Views: 683; Downloads: 460
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5.
A benchmark of lidar-based single tree detection methods using heterogeneous forest data from the alpine space
Lothar Eysn, Markus Hollaus, Eva Lindberg, Frédéric Berger, Jean-Matthieu Monnet, Michele Dalponte, Milan Kobal, Marco Antonio Pellegrini, Emanuele Lingua, Domen Mongus, Norbert Pfeifer, 2015, original scientific article

Abstract: In this study, eight airborne laser scanning (ALS)-based single tree detection methods are benchmarked and investigated. The methods were applied to a unique dataset originating from different regions of the Alpine Space covering different study areas, forest types, and structures. This is the first benchmark ever performed for different forests within the Alps. The evaluation of the detection results was carried out in a reproducible way by automatically matching them to precise in situ forest inventory data using a restricted nearest neighbor detection approach. Quantitative statistical parameters such as percentages of correctly matched trees and omission and commission errors are presented. The proposed automated matching procedure presented herein shows an overall accuracy of 97%. Method based analysis, investigations per forest type, and an overall benchmark performance are presented. The best matching rate was obtained for single-layered coniferous forests. Dominated trees were challenging for all methods. The overall performance shows a matching rate of 47%, which is comparable to results of other benchmarks performed in the past. The study provides new insight regarding the potential and limits of tree detection with ALS and underlines some key aspects regarding the choice of method when performing single tree detection for the various forest types encountered in alpine regions.
Keywords: single tree extraction, airborne laser scanning, forest inventory, comparative testing, co-registration, mountain forests, Alpine space, matching
Published: 21.06.2017; Views: 465; Downloads: 294
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6.
OLEORESINI IZ RDEČE PEKOČE PAPRIKE - EKSTRAKCIJA IN UPORABA
Jana Simonovska, 2016, doctoral dissertation

Abstract: Pepper (Capsicum annuum L.) as widely distributed vegetable crop in the world is an excellent source of nutritive and biologically active compounds. The characteristic compounds, capsaicinoids and carotenoids, highlight the importance of the red hot pepper varieties and their oleoresin extracts in the food and pharmaceutical industry. In the Ph.D. thesis was studied the possibility for a separate and integral utilization of the red hot pepper for obtaining the oleoresins from pericarp, placenta, seeds and stalk. Pre-treatment of the raw material (drying, separation of anatomical structures i.e. pericarp, placenta and seeds, and determination of theirs physico-chemical characteristics and determination of the he characteristic bioactive compounds: capsaicinoids, carotenoids and volatiles was studied, also. The second part of the Ph.D. thesis was focused of the determination of the optimal conditions for isolation of the bioactive capsaicinoids and coloured compounds, through comparative following of the thermodynamical parameters by application of organic solvents and supercritical fluids. Influence of the working parameters: temperature, time, pressure, solid to liquid phase ratio, density, type of solvents, and particle size of raw material on the yield of extract and content of capsaicinoids, colour compounds and volatiles was studied. Modelling of the experimental phase data by application of mathematical methods was performed. Re-utilization of seed and stalk from red hot pepper in form of extracts for development of new formulations as edible films, biopesticides and nanoemulsions was studied, also.
Keywords: red hot pepper, pericarp, placenta, seed, stalk, extraction, sub- and supercritical fluids, bioactive compounds, volatiles, re-utilization, edible films, biopesticides, nanoemulsions
Published: 08.11.2016; Views: 1140; Downloads: 95
.pdf Full text (4,71 MB)

7.
Subcritical water as a green medium for extraction and processing of natural materials
Matej Ravber, 2016, doctoral dissertation

Abstract: In this doctoral dissertation, the application of subcritical water as a green medium for the extraction and processing of natural materials is presented. The work is divided into three main parts. In the first part, subcritical water is proposed as a solvent for the simultaneous extraction of oil- and water-soluble phase from oily seeds. The extraction parameters, such as temperature, time and material to solvent ratio that yield the highest amounts of both phases are examined. The quality of both obtained phases is examined. The characteristics of oils obtained using subcritical water is compared to that obtained using a conventional method. The second part of this work proposes subcritical water as an efficient solvent for the isolation of bioactive phenolic compounds from wood waste, that is produced by the forestry industry. Different wood fractions are firstly extracted in batch-mode and the fraction with the highest amounts of bioactive compounds is determined. Next, semi-continuous operation is applied, where the effects of different extraction parameters are studied on the extraction yield and quality of the extract. The effect of temperature and ethanol addition to the subcritical water on the content of single phenolic compounds identified in the extracts is observed. Lastly, the cost of manufacturing of such a product is estimated by evaluating the economics of different pilot- and industrial-scale processes operating at optimal conditions determined on the laboratory scale. The last part proposes the use of subcritical water as an efficient hydrolytic medium for glycoside bonded antioxidants, specifically those found in waste agro-industrial sources. Effect of temperature, treatment time, concentration and the atmosphere used for establishing the pressure in the reactor are first studied on a model glycoside compound - rutin and the optimal combination of reaction parameters are established for the batch-mode reactor. The degradation products of the model compound are identified and the concentration/time profiles of their degradation are observed. Furthermore, the reaction kinetics explaining the degradation of the rutin standard are evaluated. In the next step, the method is implemented on a real glycosides-containing extract. The extract is hydrolyzed at conditions obtained from the first step and the free aglycone is obtained at the highest yields possible. Lastly, the process is upgraded to continuous operation and the final hydrolyzed high-purity product is recovered.
Keywords: Subcritical water, Biowaste, Extraction, Hydrolysis, Antioxidants, Hydrothermal degradation.
Published: 16.06.2016; Views: 1100; Downloads: 183
.pdf Full text (3,71 MB)

8.
Extraction of curcuminoids with subcritical water
Ignacio Macicior Borregón, 2015, undergraduate thesis

Keywords: subcritical water, extraction, curcuma
Published: 06.11.2015; Views: 991; Downloads: 46
.pdf Full text (1,47 MB)

9.
Extraction of lutein diesters from tagetes erecta using supercritical $CO_2$ and liquid propane
Mojca Škerget, Miran Bezjak, Katja Makovšek, Željko Knez, 2010, original scientific article

Abstract: The efficiency of high pressure extraction of lutein diesters from marigold (Tagetes erecta) flower petals has been investigated. The solvents used for extraction were supercritical carbon dioxide and liquid propane. Operating parameters were 300 bar and 40, 60 and 80 °C for $CO_2$ and 100, 150, 200 bar and 40 and 60 °C for propane, respectively. The influence of process parameterson the total yield of extraction and content of lutein diesters in the extracts was investigated. The results show, that solvent power of propanefor lutein diesters is approximately 3.5 times higher than of $CO_2$. The calculation procedure based on the Fick's second law was applied to determine the diffusivities of lutein diesters during extraction from marigold flower petals for both extraction stages: a constant rate stage followed by a stage of decreasing rate. The mathematical model based on the Fick's second law well described the experimental extraction results.
Keywords: lutein diesters, Tagetes errecta, extraction, supercritical $CO_2$, subcritical propane
Published: 10.07.2015; Views: 835; Downloads: 53
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10.
Detection of planar points for building extraction from LiDAR data based on differential morphological and attribute profiles
Domen Mongus, Niko Lukač, Denis Obrul, Borut Žalik, 2013, published scientific conference contribution

Abstract: This paper considers a new method for building-extraction from LiDAR data. This method uses multi-scale levelling schema or MSLS-segmentation based on differential morphological profiles for removing non-building points from LiDAR data during the data denoising step. A new morphological algorithm is proposed for the detection of flat regions and obtaining a set of building-candidates. This binarisation step is made by using differential attribute profiles based on the sum of the second-order morphological gradients. Any distinction between flat and rough surfaces is achieved by area-opening, as applied within each attribute-zone. Thus, the detection of the flat regions is essentially based on the average gradient contained withina region, whilst avoiding subtractive filtering rule. Finally, the shapes of the flat-regions are considered during the building-recognition step. A binary shape-compactness attribute opening is used for this purpose. The efficiency of the proposed method was demonstrated on three test LiDAR datasets containing buildings of different sizes, shapes, and structures. As shown by the experiments, the average quality of the buildings-extraction was more than 95%, with 96%correctness, and 98%completeness. In terms of quality, this method is comparable with TerraScan R , but both methods significantly differ when comparing correctness and completeness of the results.
Keywords: LiDAR, mathematical morphology, segmentation, DAP, DMP, building extraction
Published: 10.07.2015; Views: 858; Downloads: 335
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