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1.
FORMULATION, PREPARATION AND CHARACTERIZATION OF NANOEMULSIONS FOR PARENTERAL NUTRITION
Dušica Mirković, 2019, doktorska disertacija

Opis: The aim of this doctoral research was to develop and optimize parenteral nanoemulsions as well as the total parenteral nutrition (TPN) admixture containing a nanoemulsion obtained in the course of the optimization process (hereinafter referred to as optimal nanoemulsion), and to examine their physicochemical and biological quality as well. In addition, the quality of the prepared nanoemulsions was compared with the quality of the industrial nanoemulsion (Lipofundin® MCT/LCT 20%), and, in the end, the TPN admixture initially prepared was also compared with the admixture into which the industrial emulsion was incorporated. Parenteral nanoemulsions that were considered in this dissertation were prepared by the high-pressure homogenization method. This method is the most widely applied method for the production of nanoemulsions due to the shortest length of homogenization time, the best-obtained homogeneity of the product and the smallest droplet diameter. For the nanoemulsion formulation, preparation and optimization purposes, by using, firstly, the concept of the computer-generated fractional design, and, after that, the full experimental design, the assessment of both direct effects of different formulation and process parameters (the oil phase type, the emulsifier type and concentration, a number of homogenization cycles and the pressure under which homogenization was carried out) as well as the effects of their interactions on the characteristics of prepared nanoemulsions was performed. Monitoring the nanoemulsion physical and chemical stability parameters was carried out immediately after their preparation, and then after 10, 30 and 60 days. It included the visual inspection, the measurement of the droplet diameter (the mean and volume droplet diameter), the polydispersity index, the ζ-potential, the pH value, the electrical conductivity, and the peroxide number. After the preparation and after 60 days, the biological evaluation (the sterility test and the endotoxic test) of the prepared nanoemulsions was carried out. As far as the characterization of the TPN admixture is concerned, it included practically the same parameters. The dynamics of monitoring the characteristics of the TPN admixture was determined on the basis of practical needs of hospitalized patients (0h, 24h and 72h). The scope and comprehensiveness of this issue indicated the need to divide the doctoral dissertation into three basic stages. The first stage was preliminary. Using the 24-1 fractional factorial design, nanoemulsions for the parenteral nutrition were prepared. They contained either a combination of soybean and fish oil, or a combination of medium chain triglycerides and fish oil. In addition, the type and the amount of an emulsifier used, a number of high-pressure homogenization cycles, and the homogenization pressure, were also varied. The measurement of the above-mentioned parameters for the industrial nanoemulsion was parallely carried out (Lipofundin® MCT/LCT 20%). The objective of this part of the research was to identify critical numerical factors having the most significant effect on the characteristics that define the prepared parenteral nanoemulsions. Parameters that were singled out as the result of this stage of the research (the emulsifier concentration and a number of homogenization cycles) were used as independent variables in the second stage of the research.
Ključne besede: nanoemulsions, total parenteral nutrition admixtures, high pressure homogenization, design of experiments, optimization, analysis of variance, artificial neural networks
Objavljeno: 07.06.2019; Ogledov: 154; Prenosov: 0
.pdf Celotno besedilo (2,82 MB)

2.
Optični senzorski receptorji na osnovi azo barvil
Tinkara Mastnak, 2019, doktorska disertacija

Opis: Občutljiva in selektivna detekcija biotiolov je v zadnjih letih deležna vse večje pozornosti, saj so spremembe njihove koncentracije v krvi, plazmi in urinu povezane z različnimi obolenji. Ker ima vsaka od standardnih tehnik za njihovo detekcijo osnovne omejitve v zvezi s kompleksnostjo, pripravo vzorca, časom trajanja analize in stroški, so nove metode izjemno zaželene. Biogeni amini so vključeni v pomembne presnovne in fiziološke funkcije in so lahko naravno prisotni v hrani in pijači. Visoke vsebnosti biogenih aminov v živilih so posledica intenzivne mikrobne aktivnosti zaradi fermentacije ali kvarjenja. Tako nadzor nad biogenimi amini postaja vse pomembnejši za spremljanje procesov proizvodnje živil, za preverjanje njihove kakovosti in svežosti ter za spremljanje njihove varnosti. Podatki o prisotnosti biogenih aminov v prehrambenih izdelkih niso dosledni, ker je njihova koncentracija odvisna od vsebnosti vlage, maščob, beljakovin in pH. Te lastnosti zagotavljajo okolje za razvoj mikroorganizmov in biokemičnih reakcij, zaradi česar so živila med predelavo in skladiščenjem pokvarljiva. Določanje biogenih aminov v živilih je dolgotrajno in zahteva drage analizne instrumente. Kolorimetrična detekcija v nadprostoru tako ponuja elegantno rešitev, saj se lahko podatki povežejo s številom mikroorganizmov, s čimer posledično določimo raven svežosti ali pokvarjenosti hrane. Doktorska disertacija predstavlja lastnosti in uporabnost 4-N,N-dioktilamino-4'-dicianovinilazobenzena (CR-528) in 4-N,N-dioktilamino-2'-nitro-4'-dicianovinilazobenzena (CR-555) za zaznavanje biotiolov in biogenih aminov. Senzorne lastnosti CR-528 in CR-555 so bile najprej preizkušene v raztopini etanola. Dodajanje žveplo-vsebujočih analitov (2 merkaptoetanola (2-ME), hidrosulfida (SH─)) in določenih biogenih aminov (spermina (SP), spermidina (SPD), etanolamina (EA)) je povzročilo koncentracijsko odvisne spektralne spremembe, ki so jih spremljale vidne spremembe barve iz rožnate/vijolične do bledo rumene/oranžno-rumene. Ker detekcija omenjenih analitov v etanolu nima velike uporabne vrednosti, smo CR-528 in CR-555 imobilizirali v dve različni polimerni osnovi – hidrofilni poliuretanski hidrogel (PHD4) in hidrofobni kopolimer na osnovi etilena in vinil acetata (EVA), s čimer smo pridobili optične senzorske receptorje v obliki indikatorskih plasti. Tem smo najprej raziskali detekcijske lastnostih za zaznavanje žveplo-vsebujočih analitov (celokupnih sulfidov in 2-ME) v pufru s fiziološkim pH (7.4). Rezultati so pokazali, da je za dosego diagnostično relevantnih koncentracijskih območij potrebno močno izboljšati občutljivost indikatorskih plasti. Izkazalo se je tudi, da so samo optični senzorski receptorji na osnovi EVA dovolj stabilni, da jih je smiselno nadalje raziskati kot kolorimetrične naprave za detekcijo hlapov biogenih aminov. Reakcija CR-528/EVA in CR-555/EVA s hlapi izopentilamina (IPA) je povzročila očitno spremembo barve iz rožnate/vijolične do rumene/oranžno-rumene. CR 555/EVA optični senzorski receptor se je odzval tudi na izpostavljenost kadaverinu (CAD). Spremembe barv so bile analizirane z UV/VIS molekulsko absorpcijsko spektroskopijo, pri čemer je bila metoda delno validirana. Določili smo mejo zaznavnosti, občutljivost, linearno koncentracijsko območje, točnost in natančnost. Najnižje meje zaznavnosti so bile dosežene z CR-555/EVA (0,40 ppm za IPA in 1,80 ppm za CAD) optičnimi senzorskimi receptorji. Na zadnje smo ugotovili, da zaradi visoke reaktivnosti, neobstojnosti v raztopini v daljšem časovnem obdobju, občutljivosti na pH in na povišane temperature, barvili nista primerni za imobilizacijo v silicijeve delce.
Ključne besede: azo barvila, biogeni amini, biotioli, optični senzorski receptorji, poliuretanski hidrogel, kopolimer etilena in vinil acetata
Objavljeno: 26.04.2019; Ogledov: 347; Prenosov: 23
.pdf Celotno besedilo (7,28 MB)

3.
Celovita sinteza trajnostnih (bio)kemijskih in drugih procesnih oskrbovalnih mrež
Žan Zore, 2019, doktorska disertacija

Opis: V zadnjih letih je netrajnostni razvoj človeške družbe povzročil degradacijo okolja in velike ekonomske ter družbene probleme. Za omenjene probleme obstaja več vzrokov, poglavitna med njimi sta pospešena rast svetovnega prebivalstva in s tem vse hitrejša rast potreb prebivalstva. Za obrnitev tega trenda je pomembno, da so trenutne in nadaljnje naložbe čim bolj trajnostne. Trajnostne naložbe morajo biti sprejemljive tako iz ekonomskih, okoljskih kot socialnih vidikov. Za pravilno izbiro med trajnostnimi alternativami moramo imeti ustrezne kriterije, ki nam ponudijo rešitve, katere odražajo optimalen kompromis med gospodarsko in okoljsko učinkovitostjo ter socialno pravičnostjo. V doktorski disertaciji predstavljamo na novo razvit trajnostni kriterij ˝trajnostni dobiček˝, ki enakovredno uravnoteženo vključuje vse tri trajnostne dimenzije. Poleg ekonomskega dobička, v okoljski komponenti enakovredno obravnava neposredne obremenilne in posredne razbremenilne učinke na okolje. Socialna komponenta pa zajema vplive na zaposlene in lokalno prebivalstvo. Vsi parametri so zasnovani na monetarni osnovi, ki omogoča njihovo enostavno združevanje v končni sestavljen kriterij in je razumljiva tudi širši javnosti. Razvit trajnostni kriterij omogoča ocenjevanje naložbe tako z vidika podjetja, širše regije kot nacionalnega vidika. Določitev dolgoročnih projektov je velik izziv, zato smo trajnostni dobiček nadgradili v koncept trajnostne neto sedanje vrednosti. V doktorski disertaciji smo z novo razvitim kriterijem ˝trajnostno neto sedanjo vrednostjo˝ raziskali tudi vpliv časovne komponente na vrednotenje trajnosti. Zasnova sestavljenih kriterijev omogoča reševanje večjih sinteznih problemov, saj se večkriterijsko optimiranje z matematičnim programiranjem pri uporabi sestavljenega kriterija spremeni v enokriterijsko. Za prikaz aplikacije na novo razvitih trajnostnih kriterijev smo razvili manjši demonstracijski model energetske oskrbovalne mreže in dodelali koncept (bio)kemijske oskrbovalne mreže. Nadgradnja (bio)kemijskih oskrbovalnih mrež v širok sistem oskrbovalnih mrež predstavlja odziv na izziv izvedbe celovite večnamenske sinteze, ki temelji na trajnostnih načelih z uporabo obnovljivih virov od molekularne ravni do ravni procesnih obratov in njihovih povezav na regionalni ali celo globalni ravni. Poleg (bio)kemijske smo vključili tudi kmetijsko in energetsko oskrbovalno mrežo. Sinteza sistema oskrbovalnih mrež s svojo širino in kompleksnostjo ponuja praktično neomejeno število možnih rešitev. Ker je sinteza sistema oskrbovalnih mrež na splošno zapletena in obsežna za modeliranje, smo uporabili učinkovite dekompozicijske tehnike in tehnike za zmanjševanje velikosti modela. V okviru doktorske disertacije smo razvili metodologijo za načrtovanje novih, okolju prijaznih procesov in produktov. V povezavi z globalnim ocenjevanjem življenjskega kroga smo razvili učinkovita orodja za načrtovanje in ocenjevanje novih spojin in sintezo inovativnih procesov v procesnih industrijah. Glavna vizija koncepta je z uporabo matematičnega programiranja hkratne sinteze sistema mrež temeljito preoblikovati procese in druge sisteme, da bi dosegli trajnejšo proizvodnjo in porabo, kar ima znaten potencial za inovacije in nova odkritja.
Ključne besede: Trajnostni dobiček, trajnostna neto sedanja vrednost, trajnostni kriterij, sinteza oskrbovalnih mrež, širok sistem oskrbovalnih mrež, večnamenska optimizacija, kemijska oskrbovalna mreža, trajnostna oskrbovalna mreža
Objavljeno: 24.04.2019; Ogledov: 104; Prenosov: 23
.pdf Celotno besedilo (3,61 MB)

4.
Biomimetic membranes for forward osmosis application in industrial wastewater treatment
Jasmina Korenak, 2018, doktorska disertacija

Opis: The problem of wastewater is increasing as we face tighter regulations in limiting parameters for discharge into sewers or surface waters. At the same time, the challenge is also how to upgrade existing technology and identify new appropriate technologies for purification of industrial wastewater for re-use. The optimal solution, which can give the appropriate quality of purified water at acceptable operating costs also is not straightforward. However, increasing environmental legislative demands combined with increased fresh water consumption can facilitate implementation of emerging technologies which at the current state are not fully mature. Forward Osmosis (FO) is one such recent achievement which is considered as a promising membrane process and potentially a sustainable alternative to reverse osmosis (RO) process for wastewater reclamation and sea/brackish water desalination. However, there are many limiting parameters (e.g. membrane fouling, draw solutions) in FO process that needs to be studied and improved. To reduce the membrane fouling in FO, many improvements were attempted, e.g. synthesis of different membrane materials, fabrication of membrane modules, membrane coating etc. One of the novelties in membrane development research field is biomimetic membranes incorporate in separation processes. They employ natural proteins known as AQPs (aqpourins) to regulate the flow of water, providing increased permeability and near-perfect solute rejection. Membrane surface characteristics were measured on virgin, used and cleane membrane in order to confirm the resistance to different types of industrial wastewater and sewage.
Ključne besede: biomimetic membrane, forward osmosis, industrial wastewater, reverse osmosis, textile wastewater, ultrafiltration, wastewater reuse
Objavljeno: 25.07.2018; Ogledov: 424; Prenosov: 25
.pdf Celotno besedilo (4,64 MB)

5.
Procesi odstranjevanja antibiotikov iz bolnišničnih odpadnih vod
Severina Stavbar, 2018, doktorska disertacija

Opis: Ostanki antibiotikov in drugih zdravil, postajajo vse resnejši problem, saj jih najdemo v izpustih iz farmacevtskih in proizvodnih obratov, bolnišnic in odplakah iz čistilnih naprav. Različne študije so pokazale, da so ostanki antibiotikov prisotni v odpadnih in površinskih vodah, zadnje študije pa kažejo trend zviševanja tudi v tleh, podtalnici ter pitni vodi. Čeprav so izmerjene koncetracije v širokem koncentracijskem območju od ng/L do µg/L, so lahko nekateri razgradni produkti aktivnih snovi celo bolj toksični kot izvorna snov. Predhodne študije so pokazale, da so najvišje koncentracije antibiotikov v bolnišničnih odpadnih vodah. Za odstranitev takšnih onesnaževal pa obstoječe čistilne naprave niso primerne, saj velike količine antibiotikov ostajajo v vodi tudi po čiščenju. V doktorski disertaciji so predstavljeni trije procesi odstranjevanja teh onesnaževal iz bolnišničnih odpadnih vod. Glavni namen je bil poiskati napredne, izvedljive metode za odstranitev izbranih antibiotikov iz bolnišnične odpadne vode. V prvem delu smo se osredotočili na postopek čiščenja s sub in super-kritično oksidacijo, kjer smo preučili procesne parametre: vpliv temperature, tlaka, pretoka in časa. V drugem delu smo opravili postopek ozonacije, kjer smo spremljali učinkovitost čiščenja odpadne vode s spreminjanjem pH vzorca, različnimi odmerki ozona ter dodatek vodikovega peroksida (H2O2). V tretjem delu smo za čiščenje sintetično pripravljene bolnišnične odpadne vode uporabi aerobni reaktor, kjer smo iskali optimalen bivalni čas. Vsebnost antibiotikov smo po vsaki metodi čiščenja določali z optimiranimi LC-MS/MS analiznimi tehnikami. V zadnjem delu doktorske disertacije smo vse omenjene postopke čiščenja implementirali na realnem vzorcu bolnišnične odpadne vode. Vsebnost antibiotika v realnem vzorcu pred in po čiščenju smo določali z ekstrakcijo na trdni fazi v povezavi z optimirano LC-MS/MS tehniko. Na koncu smo izvedli še test inhibicije porabe kisika z aktivnim blatom za oksidacijo ogljika in amonija, s katerim smo poskušali ugotoviti, toksičen vpliv očiščene vode na mikrooganizme v aktivnem blatu.
Ključne besede: Antibiotiki, Bolnišnična odpadna voda, Sub-kritična oksidacija, Super-kritična oksidacija, Ozonacija, Aerobni reaktor, LC-MS/MS, Test toksičnosti
Objavljeno: 20.06.2018; Ogledov: 396; Prenosov: 73
.pdf Celotno besedilo (2,60 MB)

6.
High-Perssure process design for polymer treatment and heat transfer enhancement
Gregor Kravanja, 2018, doktorska disertacija

Opis: The doctoral thesis presents the design of several high-pressure processes involving »green solvents« so-called supercritical fluids for the eco-friendly and sustainable production of new products with special characteristics, fewer toxic residues, and low energy consumption. The thesis is divided into three main parts: polymer processing and formulation of active drugs, measurements of transport properties form pendant drop geometry, and study of heat transfer under supercritical conditions. In the first part, special attention is given to using biodegradable polymers in particle size reduction processes that are related to pharmaceutical applications for controlled drug release. The PGSSTM micronization process was applied to the biodegradable carrier materials polyoxyethylene stearyl ether (Brij 100 and Brij 50) and polyethylene glycol (PEG 4000) for the incorporation of the insoluble drugs nimodipine, fenofibrate, o-vanillin, and esomeprazole with the purpose of improving their bioavailability and dissolution rate. In order to optimize and design micronization process, preliminary transfer and thermodynamic experiments of water-soluble carriers (Brij and PEG)/ SCFs system were carried out. It was observed that a combination of process parameters, including particle size reduction and interactions between drugs and hydrophilic carriers, contributed to enhancing the dissolution rates of precipitated solid particles. In the second part, a new optimized experimental setup based on pendant drop tensiometry was developed and a mathematical model designed to fit the experimental data was used to determine the diffusion coefficients of binary systems at elevated pressures and temperatures. Droplet geometry was examined by using a precise computer algorithm that fits the Young–Laplace equation to the axisymmetric shape of a drop. The experimental procedure was validated by a comparison of the experimental data for the water-CO2 mixture with data from the literature. For the first time, interfacial tension of CO2 saturated solution with propylene glycol and diffusion coefficients of propylene glycol in supercritical CO2 at temperatures of 120°C and 150°C in a pressure range from 5 MPa, up to 17.5 MPa were measured. Additionally, the drop tensiometry method was applied for measuring systems that are of great importance in carbon sequestration related applications. The effect of argon as a co-contaminant in a CO2 stream on the interfacial tension, diffusion coefficients, and storage capacity was studied. In the third part, comprehensive investigation into the heat transfer performance of CO2, ethane and their azeotropic mixture at high pressures and temperatures was studied. A double pipe heat exchanger was developed and set up to study the effects of different operating parameters on heat transfer performance over a wide range of temperatures (25 °C to 90 °C) and pressures (5 MPa to 30 MPa). Heat flux of supercritical fluids was measured in the inner pipe in the counter-current with water in the outer pipe. For the first time, the heat transfer coefficients (HTC) of supercritical CO2, ethane and their azeotropic mixture in water loop have been measured and compared. A brief evaluation is provided of the effect of mass flux, heat flux, pressure, temperature and buoyancy force on heat transfer coefficients. Additionally, to properly evaluate the potential and the performance of azeotropic mixture CO2-ethane, the coefficients of performance (COP) were calculated for the heat pump working cycle and compared to a system containing exclusively CO2.
Ključne besede: supercritical fluids, PGSSTM, formulation of active drugs, biodegradable polymers, transport and thermodynamic data, pendant drop method, carbon sequestration, heat transfer coefficients
Objavljeno: 28.05.2018; Ogledov: 374; Prenosov: 69
.pdf Celotno besedilo (5,51 MB)

7.
Development of analytical methods for simultaneous identification and determination of phenolic compounds
Milena Ivanović, 2018, doktorska disertacija

Opis: 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.
Ključne besede: phenolic compounds, phenolic acids, extraction, GC-MS, HPLC, method optimization, deep eutectic solvents, plant material
Objavljeno: 11.04.2018; Ogledov: 534; Prenosov: 52
.pdf Celotno besedilo (5,10 MB)

8.
Formation, characterization and application of polysaccharide aerogels
Gabrijela Horvat, 2018, doktorska disertacija

Opis: The aim of this PhD dissertation was to describe and analyze the preparation and characterization of polysaccharide aerogels and their future pharmaceutical and medical application. For the research, we used four types of polysaccharides: pectin, alginate, xanthan and guar. We used two types of pectin, high-methoxyl and low-methoxyl pectin, because of their different gelation mechanisms. The first part of the dissertation describes the preparation and characterization of pure polysaccharide aerogels. First, we prepared pectin spherical aerogels, cross-linked with three different ions, and we investigated their final properties. Later, we developed a new method for the preparation of alginate, pectin, xanthan and guar aerogels. We used only ethanol and no other cross-linkers. Ethanol was removed in the later processes of supercritical drying, and the remaining final material was thus only porous polysaccharide. By this method, we were able to prepare pure xanthan and guar aerogels. Prior to this study, xanthan and guar aerogels were prepared only as composites. Pectin aerogels prepared by the new method have amazing properties. On the other hand, alginate aerogels show poor characteristics, and thus the methods need to be optimised. We tried different alginate viscosities, different alcohols (methanol, ethanol, 1-propanol and 1-butanol), and we investigated longer (24h) and shorter (1h) gel setting times. The second part of this dissertation describes the pharmaceutical and medical applications of prepared aerogels. The release of diclofenac sodium from spherical pectin aerogels was investigated in vitro. Calcium cross-linked aerogels were not able to retain the drug, and its release was immediate. In order to achieve controlled release of diclofenac sodium, zinc ions had to be used as cross-linkers. Later, a low water-soluble drug, nifedipine, was used as a model drug for the monolithic aerogels prepared by the new method. The release of nifedipine from pectin and alginate aerogels was highly increased, compared to the crystalline drug. This result is promising for future evaluation of these materials for increasing the bioavailability of poorly water-soluble drugs. Nifedipine release from xanthan and guar aerogels was prolonged up to two weeks. This result reveals a new perspective on such materials for their potential use in medicine as implants and local drug delivery. According to these results, we then developed a new coating material for medical-grade stainless steel from xanthan and pectin. An aerogel coating was loaded with diclofenac sodium and indomethacin, and their release profiles were investigated in vitro. Electrochemical analysis and cell tests proved the safety of such materials for use in medicine. Using aerogel coatings, the drug can be introduced locally into the body; therefore, the need for intravenous, post-operational treatment is greatly reduced.
Ključne besede: polysaccharides, aerogels, supercritical drying, drug carriers
Objavljeno: 09.04.2018; Ogledov: 419; Prenosov: 92
.pdf Celotno besedilo (5,84 MB)

9.
Optimizacija tvorbe filma premazov na vodni osnovi z uporabo elektrokemijske impedančne spektroskopije
Peter Berce, 2017, doktorska disertacija

Opis: Premazi na vodni osnovi predstavljajo pomemben segment v tehnologiji premazov in se uporabljajo kot okolju prijaznejša alternativa tradicionalnim premazom na osnovi organskih topil. Velika večina polimerov, ki služijo kot veziva v premazih so praktično netopna v vodi, zato se v premazih na vodni osnovi nahajajo v obliki termodinamsko nestabilne koloidne disperzije, ki je kinetično stabilizirana preko površinskega naboja in neionskih polarnih skupin. Zaradi te oblike je sušenje premazov na vodni osnovi bistveno bolj kompleksno kot sušenje tradicionalnih premazov na osnovi organskih topil. Najfleksibilnejši način optimizacije tvorbe filma iz premazov na vodni osnovi je z dodatkom koalescentov, t.j. organskih topil, ki nekaj časa zastajajo v suhem filmu in olajšajo deformacijo ter zlivanje oziroma koalescenco koloidnih delcev v homogeno polimerno plast. V doktorski disertaciji je predstavljen razvoj metodologije na osnovi uporabe elektrokemijske impedančne spektroskopije za študij tvorbe filma in optimizacijo koalescentov pri formuliranju premazov na vodni osnovi, hkrati pa so predstavljeni tudi rezultati vpliva koalescentov na lastnosti in stabilnost disperzije veziva. Naši rezultati kažejo, da koalescenti povzročajo nabrekanje in solvatacijo delcev veziva, obseg teh dveh pojavov pa je pogojen s hidrofilnostjo koalescentov, oziroma z njihovo sposobnostjo tvorjenja vodikovih vezi z vodo. Izkaže se, da je porast viskoznosti posledica povečanja volumskega dela delcev zaradi nabrekanja s topilom in zaradi znižane mobilnosti, ki jo prinese solvatacija. Koalescenti zaradi povečane solvatacije in sprememb lastnosti medija poslabšajo elektrostatično stabilnost, vendar hkrati izboljšajo sterično stabilizacijo, obseg obeh pojavov pa je zopet pogojen s hidrofilnostjo koalescenta. Razvili smo novo metodo na osnovi elektrokemijske impedančne spektroskopije, ki smo jo verificirali s pomočjo mikroskopije na atomsko silo. Preko spremembe obsega Warburgove difuzije testnega elektrolita tekom sušenja, smo kvantitativno spremljali proces tvorbe oziroma homogenizacije filma. S to novo metodo smo nato proučili vpliv hidrofilnosti, hlapnosti in količine koalescenta na tvorbo filma. Rezultati študije kažejo, da se hidrofilni koalescenti zadržujejo bližje površini delcev in tako omogočajo učinkovitejšo tvorbo filma. Ugotovili smo tudi, da do določene mere večja količina in nižja hlapnost koalescentov izboljšata tvorbo filma, vendar pa prevelika količina in uporaba prepočasnih koalescentov povzroča zastajanje topila in s tem dolgoročno mehčanje filma, ki ne doseže optimalne mehanske in kemijske obstojnosti. V disertaciji je tudi predstavljen primer optimizacije realnega zaščitenega premaza na vodni osnovi, kjer smo s pomočjo nove metode poiskali optimalno kombinacijo koalescentov in rezultate dobili desetkrat hitreje kot z uporabo klasičnih razvojnih postopkov. V doktorskem delu sta zajeta dva ključna znanstvena prispevka, in sicer nova metodologija za opazovanje in optimizacijo tvorbe filma pri premazih na vodni osnovi ter opredelitev in razlaga vplivov različnih koalescentov na stabilnost in lastnosti vodnih disperzij polimernih veziv.
Ključne besede: elektrokemijska impedančna spektroskopija, koalescent, premazi na vodni osnovi, stabilnost disperzije, tvorba filma
Objavljeno: 13.11.2017; Ogledov: 397; Prenosov: 68
.pdf Celotno besedilo (3,63 MB)

10.
Pristop za celovit nadzor izpostavljenosti nevarnim snovem na delovnih mestih
Lidija Korat, 2017, doktorska disertacija

Opis: Izpostavljenost nevarnim snovem na delovnih mestih je kompleksno področje, ki zahteva interdisciplinarno obravnavo. V doktorski disertaciji je prikazan sistemski pristop, ki problematiko obravnava celovito, tako da povezuje različne discipline, tj. splošno kemijo, analitsko kemijo, kemijsko procesno tehniko, medicino in pravo, in s tem na sistematičen način omogoča celovit nadzor nad izpostavljenostjo nevarnim snovem na delovnih mestih. Metodološki pristop je zasnovan na algoritemski način, ki sestoji iz petih korakov. V prvem koraku, »Zbiranje podatkov«, so podani napotki za učinkovito zbiranje podatkov o nevarnih snoveh oz. zmeseh na delovnih mestih, zbrane so svetovne organizacije in baze podatkov, ki zbirajo in obdelujejo te podatke. V drugem koraku, »Opredelitev nevarnosti«, so navedeni načini za prepoznavanje nevarnosti, ki izhajajo iz lastnosti nevarnih snovi oz. zmesi. Tretji korak, »Ocenitev tveganja«, prikazuje postopke za celovito obravnavo dejavnikov, ki vplivajo na tveganja in prispevajo k njihovemu zniževanju, kot so psihosocialne razmere, zdravstveni nadzor, usposabljanja, delovna oprema, delovno okolje (osvetljenost, toplotno udobje, ročno premeščanje bremen, hrup, vibracije, elektromagnetna sevanja, alkohol, droge in druge psihoaktivne snovi, ustreznost hrambe in skladiščenje nevarnih snovi), meritve kemičnih škodljivosti, osebna varovalna oprema, biološki monitoring in izvajanje notranjega nadzora. V četrtem koraku, »Ukrepi za zmanjšanje tveganja«, so opredeljeni varnostni ukrepi od tistih z najvišjo prednostjo, tj. nadomestitev nevarne kemične snovi in/ali procesa z manj nevarno ali nenevarno snovjo in/ali procesom, če je to tehnično možno, do organizacijskih in individualnih ukrepov. V petem koraku, »Revizija ocene tveganja«, so podani napotki za redno obnavljanje ocene tveganja in evalvacijo napredka. Razvito metodologijo smo prikazali na primerih delavcev, ki so izpostavljeni stirenu in svincu oz. svinčevim spojinam, na celotnem ozemlju Republike Slovenije. Izsledki raziskave kažejo, da so najvišjim koncentracijam svinca izpostavljeni delavci v proizvodnji svinčevih akumulatorjev, nekateri so izpostavljeni celo avtoriziranim svinčevim spojinam. Največji koncentraciji stirena so izpostavljeni delavci pri ročnem nanašanju poliestrskih in vinilestrskih smol, ki se jim je vrednost mandljeve kisline v urinu zvišala za 30 % v primerjavi s predhodno raziskavo. Vpliv ototoksičnosti stirena in svinca je bil v vseh dejavnostih spregledan. Preliminarno smo opredelili tudi nevarnosti za delavce, ki so izpostavljeni nanodelcem. Prednost razvite metodologije je, da predstavlja splošni postopek, ki se lahko uporabi za nadzor izpostavljenosti različnim nevarnim snovem na delovnih mestih. Rezultati disertacije so uporabni za različne ciljne skupine, kot so izpostavljeni delavci, strokovni delavci s področja varnosti, odgovorne osebe, organi nadzora, vladne strokovne službe itd. Prispevajo k zmanjšanju tveganja za obolenja in poškodbe delavcev, vplivajo na znižanje verjetnosti požara in eksplozije ter na dvig ravni kemijske varnosti. Rezultati disertacije so pokazali nekatere vrzeli na zakonodajnem področju, zato bodo potencialna podlaga za oblikovanje zakonodajnih predlogov tako v Republiki Sloveniji kot v Evropski uniji.
Ključne besede: varnost in zdravje pri delu, nadzor, nevarne snovi, stiren, svinec, biološki monitoring
Objavljeno: 09.11.2017; Ogledov: 614; Prenosov: 146
.pdf Celotno besedilo (9,86 MB)

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