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2. Kinetics of supercritical carbon dioxide extraction of borage and evening primrose seed oilPetra Kotnik, Mojca Škerget, Željko Knez, 2006, izvirni znanstveni članek Opis: In the present work, high-pressure extraction of borage (Borago officinalis L.) and evening primrose (Oenothera biennis L.) seed oil, containing the valuable -linolenic acid (GLA), has been investigated. Extraction was performed with supercritical carbon dioxide on a semi-continuous flow apparatus at pressures of 200 and 300 bar, and at temperatures of 40 and 60 °C. A constant flow rate of carbon dioxide in the range from 0.17 to 0.20 kgžhwas maintained during extraction. The extraction yields obtained using dense CO2 were similar to those obtained with conventional extraction using hexane as solvent. The composition of extracted crude oil was determined by GCanalysis. The best results were obtained at 300 bar and 40 °C for both seed types extracted, where the quality of oil was highest with regard to GLA content. The evening primrose seed oil extracted with supercritical fluid extraction was particularly rich in unsaturated fatty acidsČ up to 89.7 wt-% of total free fatty acids in the oil. The dynamic behavior of the extraction runs was analyzed using two mathematical models for describing the constant rate period and the subsequent falling rate period. Based on the experimental data, external mass transfer coefficients, diffusion coefficients and diffusivity in solid phase were estimated. Results showed good agreement between calculated and experimental data.
Ključne besede: chemical processing, high pressure technology, supecritical CO2, seed oil extraction, evening primrose, borage, free fatty acids, kinetics, modeling
Objavljeno: 31.05.2012; Ogledov: 1300; Prenosov: 62
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3. Supercritical fluid extraction of chammomile flower head flowers: comparison with conventional extraction, kinetics and scale-upPetra Kotnik, Mojca Škerget, Željko Knez, 2007, objavljeni znanstveni prispevek na konferenci Opis: Supercritical fluid extraction of chamomile flower heads was performed on semicontinuous extraction apparatus in the lab scale using carbon dioxide as solvent. The results of high pressure experiments were compared with those obtained with Soxhlet extraction, steam distillation and maceration. The obtained extracts were analysed by HPLC on ?-bisabolol, matricine and chamazulene content and by gravimetrical method on essential oil and waxes content. The highest content of active components in extracts and highest extraction yield were obtained using SFE at 250 bar and 40 °C. At this extraction conditions the two step separation was used to optimize the separation of essential oil from unwanted components. Dynamic behaviour of theSFE with single step separation runs were analysed using two mathematical models for describing the constant rate period and subsequent falling rate period. Based on the experimental data, external mass transfer coefficient, diffusion coefficient and diffusivity in solid phase were estimated. Results showed acceptable agreement of calculated and experimental data. Based on theparameters determined in the lab scale, the extraction process was successfully transferred to pilot scale.
Ključne besede: chemical processing, high pressure technology, supercritical extraction, chamomile, matricine, chamazulen, scale-up
Objavljeno: 31.05.2012; Ogledov: 1239; Prenosov: 24
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5. Phase equilibira of permethrin and dicofol with carbon dioxidePetra Kotnik, Amra Perva-Uzunalić, Mojca Škerget, Željko Knez, 2005, izvirni znanstveni članek Opis: The solubilities of pesticides (permethrin and dicofol) in CO2 were measured by a static-analytic method at pressures ranging from 10.0 MPa to 25.0 MPa andtemperatures of 293.2 K, 303.2 K, and 313.2 K. Due to the nonconventional shape of some solubility isotherms, solid-liquid transitions of pesticides under pressure of CO2 were determined using a modified capillary method. Sincethe solubilities depend on solvent density, the experimental binary solid-fluid equilibrium data were correlated as a function of solvent density by two different models.
Ključne besede: chemical processing, high pressure technology, CO2, pesticides, phase equilibria, solubility
Objavljeno: 01.06.2012; Ogledov: 1132; Prenosov: 22
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6. Phenols, proanthocyanidins, flavones and flavonols in some plant materials and their antioxidant activitiesMojca Škerget, Petra Kotnik, Majda Hadolin Kolar, Andreja Rižner Hraš, Marjana Simonič, Željko Knez, 2005, izvirni znanstveni članek Opis: Methanol extracts prepared from five plant materials native to the Mediterranean area, namely olive tree (Olea europaea) leaf, St. John's wort (Hypericum perforatum), hawthorn (Crataegus laevigata), oregano (Origanum vulgare) and laurel leaf (Lauris nobilis), were examined for their phenolic components. Total phenolic content was determined by the Folin-Ciocalteu method. The content of proanthocyanidins in acid-hydrolysed extracts was determined spectrophotometrically. The contents of free flavones (apigenin andluteolin) and flavonols (kaempferol, myricetin and quercetin) were determined by HPLC analysis. The time of hydrolysis of flavones, flavonols andproanthocyanidins was optimised. Antioxidant activities of apigenin, luteolin, kaempferol, myricetin, quercetin and of plant extracts were examined. Antioxidative activities were studied in sunflower oil at 98 °C, by measuring peroxide value, and in an aqueous emulsion system of -carotene and linoleic acid by measuring the absorbance of the sample. Among flavones and flavonols investigated, only myricetin inhibited oxidation of sunflower oil. All other flavones and flavonols showed pro-oxidative activity. Oppositely, in the emulsion system, only apigenin showed pro-oxidative activity while otherflavones and flavonols and plant extracts inhibited oxidation of -carotene.
Ključne besede: chemical processing, extraction, plant material, fenolic content, hidrolysis, antioxidants, flavones, flavonols, proanthocyanidines, oils, emulsions
Objavljeno: 01.06.2012; Ogledov: 1447; Prenosov: 76
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7. Preparation of WO[sub]3 aerogel catalysts using supercritical CO[sub]2Zoran Novak, Petra Kotnik, Željko Knez, 2004, izvirni znanstveni članek Opis: Single tungsten oxide aerogels (WO3), binary oxide aerogels (WO3-Al2O3) and ternary oxide aerogels (WO3-SiO2-Al2O3) were prepared using standard sol-gel route. Tungsten oxide tetraethoxide (WO(OCH2CH3)4) was used as the sol-gel precursor. The excellent properties of the gels obtained by the sol-gel synthesis were preserved upon supercritical drying with CO2. After supercritical drying at 40 °C and 100 bar, all aerogels were calcined to 800 °C. The influence of the synthesis parameters on the catalytic activity of WO3as supported on silica andžor alumina aerogels was investigated through thetransformation of N-(phosphonomethyl)iminodiacetic acid to N-(phosphonomethyl)glycine. Despite including WO3 into single and mixed silicaand alumina aerogels, high specific surface areas (284-653 m2 g-1) were preserved. Higher conversion was obtained for catalysts with higher ratios of WO3 in the mixed silica-alumina aerogels that were calcined at 800 °C.
Ključne besede: chemical processing, aerogels, catalysts, tungsten oxides, preparation of aerogels, characterisation of aerogels, supercritical CO2, supercritical drying, high pressure technology
Objavljeno: 01.06.2012; Ogledov: 1188; Prenosov: 20
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8. Phase equilibria in systems containing [alpha]-tocopherol and dense gasMojca Škerget, Petra Kotnik, Željko Knez, 2003, izvirni znanstveni članek Opis: Solubility of ▫$alpha$▫-tocopherol in CO2 and propane was determined at temperatures 303, 313, 333 and 353 K and over a pressure range from 79 to 286 bar for CO2 and 16 to 112 bar for propane. A static-analytic method was applied. The solubility of ▫$alpha$▫-tocopherol in dense CO2 under the conditions investigated was in the range of 0.2-17.0 mg/g CO2. The maximal solubilities of ▫$alpha$▫-tocopherol in propane were approximately up to ten times higher than in CO2 and were in the range from 38.9 to 171.9 mg/g propane. Phase equilibrium data for Milk Thistle seed oil in supercritical CO2 were determined at temperatures 313, 333 and 353 K and pressures ranging from 100 to 300 bar. The oil was previously additionally vitaminized and contained 1.9 wt.% of ▫$alpha$▫-tocopherol and 1.7 wt.% of free fatty acids (FFA). The solubility of oil in CO2 was in the range from 1.3 to 17.9 mg/g CO2. The distribution coefficients of ▫$alpha$▫-tocopherol and FFA between light and heavy phase were determined on a solvent free basis. The obtained separation factors increased with temperature and pressure to approximately 160-200 bar and decreased with a further increase of pressure.
Ključne besede: chemical processing, supercritical fluids, phase equilibria, separation factors, vitamin E, CO2, dense gases
Objavljeno: 01.06.2012; Ogledov: 1081; Prenosov: 19
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9. Ekstrakcija biološko aktivnih komponent iz industrijske konopljeTeo Makoter, 2019, diplomsko delo Opis: Industrijska konoplja (Cannabis Sativa L.) znova pridobiva svoj pomen v svetu kmetijstva in zdravstva. V zadnjih nekaj letih je pridelovanje industrijske konoplje in izdelkov iz nje zelo naraslo. Danes lahko najdemo veliko kmetij, ki industrijsko konopljo redno pridelujejo in prodajajo njeno seme, listje, cvetje in tudi izdelke, pridelane iz nje, kot so eterična olja in smole.
V diplomskem delu smo raziskali različne načine izločanja kanabinoidov in ostalih biološko aktivnih komponent iz posušenih in zmletih lističev industrijske konoplje. Poskusili smo ekstrahirati kanabinoide, kot so CBD, CBN, CBC in njihove kisline CBDA ter CBGA. Našteti kanabinoidi se velikokrat pojavljajo tako v zdravstvu, kot tudi pri osebni uporabi. Raziskave kažejo, da naj bi predvsem CBD in CBG imela pozitiven učinek pri zmanjševanju bolečin in zdravljenju raka.
Kanabinoide smo ekstrahirali s konvencionalnimi metodami z uporabo različnih topil in z nekonvencionalnimi metodami z uporabo superkritičnega ogljikovega dioksida (CO2). Izvedli smo ekstrakcije s Soxhletovo aparaturo, ultrazvočne ekstrakcije in maceracije z uporabo različnih topil; metanola, etanola in heksana. Ekstrakcije s superkritičnim CO2 smo izvedli v avtoklavu pri različnih temperaturnih in tlačnih pogojih, pri nekaterih smo uporabili tudi kotopilo metanol.
Ekstrakte smo nato analizirali z LC-MS metodo, kjer smo določili vsebnost posamezne kanabinoidne komponente. S Clevengerjevo metodo smo izolirali eterično olje iz industrijske konoplje ter s pomočjo GC-MS določili prisotnost terpenskih komponent.
S Clevengerjevo metodo smo poskusili pridobiti nekaj eteričnega olja, izkoristek je bil majhen, saj smo pridelali 0,4 ml olja iz 30 g konoplje.
Ključne besede: konoplja, kanabinoidi, konvencionalna ekstrakcija, superkritična ekstrakcija, LC-MS, eterično olje
Objavljeno: 19.07.2019; Ogledov: 450; Prenosov: 120
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10. Načrtovanje visokotlačne separacije maščobnih kislin iz rastlinskih oljPetra Kotnik, 2014, doktorska disertacija Opis: Predstavljeno delo obravnava raziskave na področju faznih ravnotežij, ekstrakcije in frakcioniranja maščobnih kislin v rastlinskih oljih, obogatenih s prostimi maščobnimi kislinami (FFA) pri visokih tlakih v inertnem mediju, kot je ogljikov dioksid (CO2). Podatki so ključni za nadaljnje načrtovanje visokotlačnih separacijskih procesov, saj pripomorejo k izboljšanju določenih industrijskih procesov v smeri okoljevarstva in kvalitete proizvodov. Baze podatkov že vsebujejo podatke faznih ravnotežij za sistem rastlinska olja – CO2. Zaradi širokega izbora rastlinskih olj, ki se danes nahajajo na tržišču, podatki o faznih ravnotežjih za vsa olja niso dostopni. Predvsem v literaturi ni podatkov za fazna ravnotežja pri tlakih višjih od 350 bar in podatkov o faznih inverzijah v sistemih rastlinsko olje – CO2. Delo je tako omejeno na tri rastlinska olja, ki so komercialno dostopna, to so repično olje, olje koruznih kalčkov in olje boraga. Olja so predhodno obdelana s postopkom umiljenja in na ta način obogatena s prostimi maščobnimi kislinami. Meritve faznih ravnotežij in opazovanja faznih inverzij so izvedena na sistemih FFA-obogateno repično olje – CO2, FFA-obogateno olje koruznih kalčkov – CO2 in FFA-obogateno olje boraga – CO2 v območju tlakov med 100 in 550 bar in temperaturah 35, 45, 65 in 85 °C. Vsebnost maščobnih kislin smo določili s plinsko kromatografijo in na podlagi dobljenih rezultatov določili porazdelitvene koeficiente in separacijske faktorje.
Raziskave visokotlačne ekstrakcije olja iz semen s CO2 smo izvedeli na dveh naravnih materialih z visoko vsebnostjo prostih maščobnih kislin, to so semena boraga (Borago officinalis L.) in semena nočnega svetlina (Oenthera biennis L.) pri tlaku 200 in 300 bar in temperaturah 40 in 60 °C. Ekstrakcijske krivulje smo ovrednotili z dvema matematičnima modeloma, ki kar najbolje opišeta potek ekstrakcijske krivulje v območju stacionarnega prenosa snovi in v območju nestacionarnega prenosa snovi.
Zaključek raziskave predstavlja frakcioniranje repičnega olja v smeri izolacije -linolenske kisline in koncentriranja FFA in -sitosterola v oljih. Pri koncentriranju FFA smo uporabili dva postopka, prvi je superkritična ekstrakcija v dveh stopnjah, ki daje zadovoljive rezultate v primerjavi s konvencionalno metodo kolonske kromatografije.
Ključne besede: fazno ravnotežje, ekstrakcija, separacija, ogljikov dioksid, rastlinska olja, proste maščobne kisline, beta-sitosterol, gamma-linolenska kislina
Objavljeno: 12.06.2014; Ogledov: 1347; Prenosov: 175
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