20.500.12556/DKUM-81915 Formulacija kompozitov z resveratrolom s superkritičnimi fluidi magistrsko delo Preparation of resveratrol-loaded composites with supercritical fluids Magistrsko delo obsega raziskave termodinamskih in transportnih lastnosti učinkovine resveratrol v sistemu s superkritičnim argonom. Cilj raziskav je bil pridobiti podatke, pomembne za načrtovanje in optimizacijo visokotlačnih procesov za pridobivanje delcev in kompozitov s superkritičnimi fluidi. S statično-analitično metodo smo določili topnosti resveratrola v argonu pri temperaturah 40 ºC in 60 ºC v tlačnem območju med 50 bar in 400 bar. Uporabili smo visokotlačno optično celico s spremenljivim volumnom. Vsebnost aktivne učinkovine v vzorcih smo določili spektrofotometrično. Rezultate smo predstavili grafično v obliki topnostnih izoterm. Ugotovili smo, da topnost resveratrola v argonu z naraščanjem tlaka pri konstantni temperaturi narašča in z naraščanjem temperature pri konstantnem tlaku pada. V splošnem je topnost resveratrola v argonu majhna. Najvišja izmerjena topnost je bila 8,0·10-7 g resveratrola /g argona. V nadaljevanju smo določili tališča resveratrola v argonu pri različnih tlakih. Za določanje tališča smo uporabili modificirano kapilarno metodo. Meritve smo izvedli v območju tlaka, kjer se argon obnaša kot superkritični fluid, tj. od 50 bar do 350 bar. Rezultate smo predstavili grafično v obliki talilne krivulje. Ugotovili smo, da temperatura tališča s tlakom pada. Talilna krivulja kaže negativen odklon dp/dT, kar govori o relativno dobri topnosti argona v talini resveratrola. Za konec smo izvedli še šaržno mikronizacijo resveratrola s polimernim nosilcem Brij S100 z uporabo visokotlačnega PGSSTM procesa v prisotnosti superkritičnega argona. Preučili smo vpliv tlaka in masnega razmerja resveratrol/Brij S100 na izkoristek in učinkovitost procesa. Mikronizacijo smo izvedli pri temperaturi 60 ºC in tlakih 100 bar in 200 bar za dve masni razmerji (2g/20g in 4g/20g). Za kvantitativno analizo vsebnosti resveratrola v formuliranih kompozitnih delcih smo uporabili LC-MS metodo. Ugotovili smo, da so se pridobljeni kompozitni delci pri vseh pogojih aglomerirali. Vpliv tlaka in masnega razmerja pa nimata večjega vpliva na izkoristek in učinkovitost procesa. Izkoristki procesov se gibljejo med 56,3 % in 61 %, učinkovitosti vgrajevanja učinkovine v polimerni nosilec pa med 31,6 % in 35,9 %. The master's thesis comprises research on the thermodynamic and transport properties of the active ingredient resveratrol in the system with supercritical argon. The aim of the research was to obtain the data that is important for the design and optimization of high-pressure processes to form the particles and composites with supercritical fluids. Solubility of resveratrol in argon was determined at temperatures of 40 ºC and 60 ºC in the pressure range between 50 bar and 400 bar using a static-analytical method. A high-pressure optical cell with a variable volume was used. The content of the active substance in the samples was determined spectrophotometrically. The results are presented graphically in the form of solubility isotherms. It was found that the solubility increases with increasing pressure at a constant temperature and decreases with increasing temperature at a constant pressure. The solubility of resveratrol in argon is generally low. The highest measured solubility was 8,0·10-7 g resveratrol/g argon. The melting points of resveratrol in argon at different pressures were also determined using a modified capillary method. The measurements were determined in the pressure range from 50 bar to 350 bar. The results are represented graphically in the form of a melting curve. It was found that the melting temperature decreases with pressure. The melting curve shows a negative dp/dT slope, which indicates a relatively good solubility of argon in the resveratrol melt. Additionally, batch micronization of resveratrol with a polymer carrier (Brij S100) using a high-pressure PGSSTM process was performed. The impact of the pressure and mass ratio of resveratrol/Brij S100 on the efficiency of the process was studied. The micronization was performed with argon at a temperature of 60 ºC and pressures of 100 bar and 200 bar for two mass ratios (2g/20g, 4g/20g). The LC-MS/MS method was used for a quantitative analysis of the resveratrol content in the formulated composite particles. It was determined that the obtained composite particles agglomerated under all conditions. The impact of the pressure and mass ratio does not have a significant impact on the efficiency/yield of the process. The efficiencies of the processes varies between 56,3 % and 61 %, and the efficiency of loading the active ingredient into the carrier between 31,6 % and 35,9 %. resveratrol Brij S100 argon termodinamske lastnosti PGSS proces resveratrol Brij S100 argon thermodynamic properties PGSS process true true false [N. Kotnik] Slovenski jezik Angleški jezik Magistrsko delo/naloga 2022-06-17 12:22:46 2022-07-12 14:23:04 2022-08-10 00:59:09 0000-00-00 00:00:00 2022 0 Maribor 0 Maribor 1 spletni vir (1 datoteka PDF (XI, 50 f.)) 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 544.3-139:620.168(043.2) 116185603 MAG_Kotnik_Nusa_2022.pdf MAG_Kotnik_Nusa_2022.pdf 1 53E389B3F12130ED08FC420B99E52529 db9b71b2c7e7989ea700aa53095b39e36b26998ec18fd949f112bfd2a9c4c60b b2e8d72d-01c5-11ed-9540-00155d000105 20.500.12556/dkum/17df806d-a38c-4104-b329-048fde3085e0 https://dk.um.si/Dokument.php?lang=slv&id=159336 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0