1. Synergistic effect of supercritical and ultrasound-assisted ginger (Zingiber officinale Roscoe) extractsTaja Žitek Makoter, Nika Kučuk, Vesna Postružnik, Maja Leitgeb, Željko Knez, Mateja Primožič, Maša Knez Marevci, 2022, original scientific article Abstract: Proper processing of natural material is crucial to obtain an extract with high content of
biologically active components. Dried, grinded ginger roots were extracted by ultrasonic method
and supercritical extraction with CO2
. The aim of the study was to determine if a mixture of the two
types of extracts attained by different methods and solvents exhibits better bioavailability than each
extract itself. Therefore, both extracts were analytically evaluated and then mixed in a ratio of 1:1.
The supercritical extract (SCG extract) and the mixed extract (mixG extract) had high antioxidant
activity (78% and 73%) and total phenols (827 mg/g ext. and 1455 mg/g ext.), which is also consistent
with the levels of gingerol (303 mg/g ext. and 271 g/g ext.) and shogaol (111 mg/g ext. and 100 g/g
ext.) in the extracts. In comparison to both pure extracts higher levels of total phenols were found
in the extract mixG. This could be the reason for the significant inhibition of melanoma cells and
antimicrobial potential (against Staphylococcus aureus, Escherichia coli, and Candida albicans). The
combination of the extracts resulted in a significant increase in the inhibition of selected microbial
and melanoma cells WM-266-4 compared to the control. Cell viability decreased below 60% when
mixG extract was applied. Antimicrobial activity has been confirmed. Keywords: ginger, supercritical fluid extraction, ultrasound-assisted extraction, antimicrobial activity Published in DKUM: 09.05.2025; Views: 0; Downloads: 2
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2. Optimisation of the green process of industrial hemp - preparation and its extract characterisationTaja Žitek Makoter, Petra Kotnik, Teo Makoter, Vesna Postružnik, Željko Knez, Maša Knez Marevci, 2022, original scientific article Abstract: Natural medicines and products are becoming increasingly important in the pharmaceutical
and food industries. The most important step in obtaining a natural remedy is the processing of
the natural material. This study offers the separation of the industrial hemp plant into fractions by
mechanical treatment, which has a significant impact on the selectivity of the obtained fractions. This
study also offers a solution to reduce waste by fractionating industrial hemp, focusing on the fraction
with the highest cannabinoid content (49.5% of CBD). The study confirmed the anticancer potential
of the extract, which prevents further division of WM-266-4 melanoma cells at a concentration of
10−3 mg/mL. However, application of the extract (c = 10−3 mg/mL) to normal human epidermal
melanocytes proved to be insignificant, as the metabolic activity of the cells was the same as in the
control cell group. Keywords: supercritical fluid extraction, ultrasonic extraction, melanoma cells, extraction, WM-266-4 Published in DKUM: 09.05.2025; Views: 0; Downloads: 2
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3. Optimization of the supercritical extraction and decarboxylation process of industrial hempTaja Žitek Makoter, Petra Kotnik, Teo Makoter, Željko Knez, Maša Knez Marevci, 2025, original scientific article Abstract: Cannabinoids are the main active ingredients of Cannabis sativa L., obtained by a suitable extraction method and decarboxylation, in which the acid forms of the cannabinoids are converted into active forms. Supercritical CO2 extraction method and decarboxylation process were optimized for 7 cannabinoids (CBD, CBDA, THC, THCA, CBGA, CBN and CBC). The optimal extraction conditions for all cannabinoids were determined at a temperature of 60 °C and a pressure of 300 bar to 550 bar. At higher temperatures and reaction times, a significant depletion of neutral cannabinoids was observed. The optimal conditions of the decarboxylation process varied depending on the component. For the CBD component, which could be measured in the highest concentrations (560 mg/g), the optimal conditions were 140 °C and 10 min. The study can be an important model for predicting the behavior of cannabinoids under certain parameters. Keywords: supercritical fluids, extraction, cannabinoids, decarboxilation, Cannabis sativa I Published in DKUM: 08.01.2025; Views: 0; Downloads: 7
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5. Extraction of active compounds from mixtures of hemp (Cannabis sativa) with Pants of the Zingiberaceae familyVesna Postružnik, Taja Žitek Makoter, Darko Goričanec, Petra Kotnik, Željko Knez, Maša Knez Marevci, 2023, original scientific article Keywords: supercritical fluid extraction, ultrasound-assisted extraction, hemp, ginger, turmeric, cardamom Published in DKUM: 08.05.2024; Views: 234; Downloads: 20
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6. Green techniques for preparation of red beetroot extracts with enhanced biological potentialDragana 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: 436; Downloads: 125
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7. Sustainable processing of materials using supercritical fluids : doktorska disertacijaDragana 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: 1029; Downloads: 144
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8. Extraction and separation of active compounds by supercritical fluids extraction and preparative supercritical chromatographyAlejandro 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: 2243; Downloads: 255
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9. OLEORESINI IZ RDEČE PEKOČE PAPRIKE - EKSTRAKCIJA IN UPORABAJana 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 in DKUM: 08.11.2016; Views: 2255; Downloads: 178
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10. Extraction of lutein diesters from tagetes erecta using supercritical $CO_2$ and liquid propaneMojca 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 in DKUM: 10.07.2015; Views: 1514; Downloads: 143
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