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FTIR-spektroskopische Untersuchungen zum Aktivierungsmechanismus von bovinem und humanem RhodopsinKazmin, Roman 13 August 2015 (has links)
Das aus dem Apoprotein Opsin und dem kovalent gebundenen Liganden bestehende Rhodopsin dient als Modellsystem für den Aktivierungsmechanismus der größten Klasse von G-Protein-gekoppelten Rezeptoren (GPCR). Infolge einer photochemischen Reaktion vollführt Rhodopsin eine Bewegungsabfolge von Sekundärstrukturelementen, wodurch es aktiviert wird, das G-Protein bindet und den Stimulus auf zellinterne Signalwege überträgt. Mithilfe der ortsspezifischen Mutagenese wurden Mutanten des bovinen Rhodopsins erzeugt, in eine künstliche Lipidumgebung eingelagert und hauptsächlich mittels FTIR-Spektroskopie untersucht. Anhand der Y191F- und Y192F-Mutanten konnte die Translokation des transienten Gegenions der Schiffschen Base Glu181 während der Aktivierung bestimmt werden. Die Interaktionen des Tyr206 sind für die gekoppelte Bewegung von EL2 und TM5 mitbestimmend, was mittels Y206F-Mutante gezeigt wurde. Eine Anhäufung von Methioninen auf der cytoplasmatischen Seite des Rezeptors ist u.a. für das Ausklappen der TM6 zuständig. Diese Bewegung ist wichtige Determinante der Rezeptoraktivierung. Hierfür wurden insgesamt fünf Mutanten verwendet. Im zweiten, hauptsächlichen Teil der Arbeit wird das bislang kaum untersuchte humane Rhodopsin mit dem bovinen Rezeptor verglichen. Ausgehend von verschiedenen Dunkelzuständen, konnte gezeigt werden, dass die Aktivierungsmechanismen beider Rezeptoren voneinander divergieren, um letztlich bei der Bildung der aktiven Spezies wieder zu konvergieren. Über die Analyse der Aminosäuresequenzen der Mammalia-Rhodopsine wurden zwei Bereiche hoher Variabilität identifiziert, die u.a. die molekulare Ursache für diese Diskrepanzen liefern. Diese Feststellung wurde mit human-bovinen-Rhodopsinchimären bewiesen. Ergänzend zu dieser Studie wurde Schafsrhodopsin einem Vergleich sowohl mit bovinem als auch mit humanem Rezeptor unterzogen. Es zeigte, als eine weitere natürlich vorkommende Variante des Lichtrezeptors, einen eigenständigen Weg der Aktivierung. / Rhodopsin, which consists of the apoprotein opsin and its covalently bound ligand, is used as a model system to understand the activation mechanism of the large family of G protein coupled receptors (GPCRs). As a result of a photochemical reaction, rhodopsin undergoes activating structural changes, enabling it to bind the G protein and transmitting the stimulus to intracellular signaling pathways. In the first part of this work, site-directed mutants of bovine rhodopsin were produced, incorporated into an artificial lipid environment, and studied mainly by FTIR spectroscopy. The translocation of the transient Schiff base counterion (Glu181) during the activation process was determined using the Y191F- and Y192F-mutants. The interactions of Tyr206 contributed to the coupled movement of EL2 and TM5, which was shown by Y206F-mutant. A striking accumulation of methionines on the cytoplasmic side of the receptor was observed to be a key-player for the activating outward motion of TM6. In the second and primary part of this work, human rhodopsin, which has been rarely studied, was compared with the bovine receptor. Starting from various dark states, it was shown that the activation mechanisms of both receptors diverge from each other and yet ultimately converge in the formation of the active species. By analyzing the amino acid sequences of mammalian rhodopsins, two regions of high variability were identified, which provide the molecular basis for these discrepancies. This finding was verified by the investigation of human/bovine rhodopsin chimeras. In addition to this study, ovine rhodopsin was compared with both the bovine and human forms. It showed, as another naturally occurring variant of the light receptor, an independent pathway of activation.
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Structural and spectroscopical study of crystals of 1,3,4-oxadiazole derivatives at high pressureFranco González, Olga January 2002 (has links)
Die Suche nach neuen Materialien von technischem Interesse hat in den letzten Jahren neue Antriebe zu der Untersuchung organischer Verbindungen gegeben. Organische Substanzen haben viele Vorteile wie z.B. die Möglichkeit, ihre Eigenschaften durch verschiedene chemische und physikalische Techniken im Herstellung-Prozess für ein bestimmtes Ziel zu modifizieren. Oxadiazolverbindungen sind interessant aufgrund ihrer Nutzung als Material für Licht emittierende Dioden und Scintillatoren. <br />
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Die physikalischen Eigenschaften eines Festkörpers hängen von seiner Struktur ab. Unterschiedliche Strukturen entwickeln unterschiedliche intra- und intermolekülare Wechselwirkungen. Eine ausgezeichnete Weise, um sowohl die intra- als auch die intermolekularen Wechselwirkungen eines bestimmtes Stoffes zu beeinflussen, ohne seine chemischen Charakteristiken zu ändern, ist die Verwendung von hohem Druck. <br />
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Wir haben den Einfluss von hohem Druck und hoher Temperatur auf die super-molekulare Struktur einiger Oxadiazolverbindungen im kristallinem Zustand untersucht. Aus diesen Untersuchungsergebnissen wurde eine Zustandsgleichung für diese Kristalle bestimmt. Überdies wurden die spektroskopischen Eigenschaften dieser Materialien unter hohem Druck charakterisiert. / In recent years the search for new materials of technological interest has given new impulses to the study of organic compounds. Organic substances possess a great number of advantages such as the possibility to adjust their properties for a given purpose by different chemical and physical techniques in the preparation process. Oxadiazole derivatives are interesting due to their use as material for light emitting diodes (LED) as well as scintillators. <br />
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The physical properties of a solid depend on its structure. Different structures induce different intra- and intermolecular interactions. An advantageous method to modify the intra- as well as the intermolecular interactions of a given substance is the application of high pressure. Furthermore, using this method the chemical features of the compound are not influenced.<br />
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We have investigated the influence of high pressure and high temperature on the super-molecular structure of several oxadiazole derivatives in crystalline state. From the results of this investigation an equation of state for these crystals was determined. Furthermore, the spectroscopical features of these materials under high pressure were characterized.
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Neuartige höherkoordinierte Siliciumkomplexe mit Pyrrol-2-carbaldimin-LigandenGerlach, Daniela 01 February 2013 (has links) (PDF)
Im Rahmen dieser Arbeit wurden Siliciumkomplexe mit dianionischen Pyrrol-2-carbaldimin-funktionalisierten N,N,O- und N,N,N,N-Chelatliganden synthetisiert und kristallografisch, NMR- und UV/Vis-spektroskopisch und mittels quantenchemischer Berechnungen charakterisiert. Die pentakoordinierten Si-Komplexe mit N,N,O-Ligandrückgraten wiesen in Abhängigkeit von den weiteren Si-gebundenen Substituenten unterschiedlich konfigurierte verzerrt trigonal-bipyramidale Si-Koordinationssphären auf. Die Ursache der Farbigkeit dieser Verbindungen konnte mittels quantenchemischer Berechnungen detailliert erklärt werden. – Die Si-Komplexe mit N,N,N,N-Ligandrückgraten liegen in Abhängigkeit von den weiteren Si-gebundenen Substituenten als 5-fach koordinierte kationische oder neutrale 6-fach koordinierte Si-Komplexe vor. Deren Farbigkeit wurde mittels UV/VIS-Spektroskopie untersucht. Von ausgewählten Komplexen wurden die Tensoren der 29Si-NMR-Verschiebung rechnerisch und CP/MAS-NMR-spektroskopisch bestimmt.
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Application of Hot-Melt Ink Jet Processes for Imaging at Offset Printing Form CylinderAbd El Kader, Magdy Ezzat 30 January 2004 (has links) (PDF)
The present work related to apply hot-melt ink-jet process for imaging at offset lithographic printing form, to utilise a reusable surface for many times and particularly related to validating thermal and ultrasonic erasing processes. This dissertation investigated systematically the role of certain factors towards affecting erasing image area process on print surfaces. Thermal erasing process approved to melt and suck the image area from the surface, the results were adopted by using contact angle measurements and scanning electron microscope. Ultrasonic erasing process permitted to solve the image area by choosing erasing chemistries, influence of selected erasing chemistries on printing surface, and evaluation the process, the results were tested by UV/Vis spectrometer, contact angle, profileometery and visual microscope. / Der Fortschritt im Bereich von Charakterisierung und
Verständnis für Hot-melt Ink Jet Prozesse zur Bebilderung von Offsetdruckform-Zylindern ist ein Ergebnis dieser Forschung.
Die Systematik dieser Arbeit basiert auf einem theoretischen Teil, um einen geeigneten Löschprozess auszuwählen. Der Löschprozess hängt von den Eigenschaften des Hot-melt Ink Jet Materials und der genutzten Aluminiumdruckoberfläche ab. Diese werden systematisch im Labormaßstab experimentell untersucht. Der thermische Prozess wurde einerseits durch Benetzbarkeitsprüfungen und anderseites durch Rasterelektronmikroskopaufnahmen bewertet.Der Ultraschallprozess ist ein nasser Löschprozess. Die Untersuchungen wurden in vier Stufen systematisch durchgeführt
- Auswahl vom geeigneten Lösungsmitteln
- Einflüsse von ausgewählten Lösungsmitteln auf nicht beschichtete und beschichtete Aluminium platten
- Evaluation eines Ultraschalllöschprozesses
- Validation eines Löschprozesses; zur Bewertung des Löschprozesses wurden mehrere Druckplattenproben bebildert und gelöscht
Die Ergebnisse wurden durch UV/Vis Spektrometer, Kontaktwinkel, Profiliometrie und Visuelle Mikroskopie getestet.
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Protein phosphatase biosensor for the detection of cyanotoxins associated with algal bloomMniki, Nontle Catherine January 2013 (has links)
Magister Scientiae - MSc / The toxicity of microcystin is associated with the inhibition of serine/threonine protein phosphatases 1 and 2A, which can lead to hepatocyte necrosis and haemorrhage. Analysis of microcystin is most commonly carried out using reversed-phase high performance liquid chromatographic methods (HPLC) combined with ultra-violet (UV) detection .The ability of these techniques to identify unknown microcystin in environmental samples is also restricted by the lack of standard reference materials for the toxins. Highly specific recognition molecules such as antibodies and molecularly imprinted polymers (MIPs) have been
employed in the pre-concentration of trace levels of microcystin from water and show great potential for the clean-up of complex samples for subsequent analysis. New biosensor technologies are also becoming available, with sufficient sensitivity and specificity to enable rapid ‗on-site‘ screening without the need for sample processing. In this work we constructed a Protein phosphatase biosensor for detection of microcystin-LR in aqueous medium, onto polyamic acid/graphene oxide (PAA: GO) composite electrochemically synthesised in our laboratory. The composites were synthesised at three different ratios i.e. 50:50, 80:20 and 20:80 to evaluate the effect of each component in the search to produce highly conductive mediator platforms. The electrochemistries of the three different composites were evaluated using CV and SWV to study interfacial kinetics of the
materials as thin films at the glassy carbon electrode. The phosphatase biosensor parameters were evaluated using CV, SWV, EIS and Uv-vis spectroscopy. The affinity binding of the microcystin-LR to protein phosphatase 2A was investigated using electrochemical impedance spectroscopy which is a highly sensitive method for measuring interfacial kinetics of biosensor systems.
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Determinação espectrofotométrica do teor de biodiesel metílico em misturas com óleo diesel / Spectrophotometric determination of methyl biodiesel content in blends with dieselSILVA, Marcos Alexandro Abreu e 25 November 2009 (has links)
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Previous issue date: 2009-11-25 / In this work it was developed a quantitative analytical methodology to determine the content of methyl biodiesel in diesel fuel through the fatty acid methyl ester reaction with the hydroxylamine hydrochloride in alkaline solutions, which they were acidified and converted to hydroxamic acids, followed by treatment with ferric ion to give the colored ferric hydroxamate complex, and afterwards extract in n-heptane and were analysed by UV-visible spectroscopy. It was made the optimization of the variables that interfere in the reaction, and parameters such as accuracy, precision and the limit of detection (LOD) among other parameters to assess the quality of the method developed it was also evaluated. The results indicated that the method has shown an excellent linearity in small intervals of biodiesel blend levels, an excellent determination coefficient of the calibration curve (R2 > 0.99) at a wide range of wavelength (420-440 nm). As well as it has also shown to be applied in a wide range of methyl biodiesel blend levels in diesel fuel (B1 to B20), and it is suitable to be used in the quality control procedures for the production of BX blends. / Desenvolveu-se neste trabalho uma metodologia analítica quantitativa para determinação do teor de biodiesel metílico em óleo diesel por meio da reação dos ésteres metílicos de ácidos graxos com o cloridrato de hidroxilamina em meio alcalino, os quais são acidificados e convertidos à ácidos hidroxâmicos, seguida pelo tratamento com íons ferro (III) resultando em complexos coloridos de hidroxamato férrico, posteriormente extraídos em n-heptano e analisados por espectroscopia de UV-visível. Fez-se a otimização das variáveis que interferem na reação, e também avaliou-se a exatidão, precisão, e o limite de detecção (LD), entre outros parâmetros, no sentido de avaliar a qualidade do método desenvolvido. O método mostrou excelente linearidade em pequenos intervalos de variação volumétrica de biodiesel, excelente coeficiente de correlação para a curva de calibração (R2 > 0,99), em uma ampla faixa de comprimento de onda (420 a 440 nm). Assim como mostrou ser aplicável em uma ampla faixa de teor de biodiesel metílico em óleo diesel (B1 ao B20), sendo adequado para o controle de qualidade da produção de misturas BX.
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Dispersionsoptimierung von Kohlenstoffnanoröhren für die Herstellung von Polymer-Komposit-Drucksensoren / Optimization of carbon nanotubes dispersions for polymer composite-based pressure sensorsGerlach, Carina 27 November 2017 (has links) (PDF)
Kohlenstoffnanoröhren (engl. carbon nanotubes, CNT)-Polymer-Komposite haben ein großes Potential im Bereich sensorischer Anwendungen. Dabei spielen die elektrischen Eigenschaften des Komposits und deren Änderungen unter mechanischer Belastung eine entscheidende Rolle. Einen maßgeblichen Einfluss nimmt dabei das Aspektverhältnis der CNT-Agglomerate sowie der CNTs selbst ein, welches jeweils vom CNT-Desagglomerationsprozess bestimmt wird. Die Dispergierung beeinflusst folglich auch die elektrische Leitfähigkeit und Reproduzierbarkeit des Komposits sowohl im mechanisch unbelasteten als auch belasteten Zustand. Dies wurde anhand von (teil-)analytischen Modellen gezeigt.
Die Dispersionsqualität wird dabei von vielen Faktoren beeinflusst, wobei die Prozessparameter beim Ultraschalldispergieren derzeit nach der Trial-and-Error-Methode bestimmt werden. Im Rahmen der Arbeit wurde eine Dispergiergleichung für zylindrische Partikel, die CNTs näherungsweise sind, erstmals für die Dispergierung von CNTs in Lösungsmitteln entwickelt, angewendet sowie verifiziert. Die Gültigkeit der Gleichung für CNTs wurde durch Variation der Ultraschallparameter Zeit sowie Energie und deren Einfluss auf den Dispergiergrad gezeigt. Die mittels UV-VIS-Spektroskopie gemessene Extinktion diente dabei als indirekte Messgröße des Dispergiergrads. Nach Vorversuchen zur geeigneten Materialauswahl wurden alle relevanten Einflussparameter berechnet oder experimentell bestimmt. Die experimentelle Verifikation erfolgte an CNT-N-Methyl-2-pyrrolidon-Dispersionen, die mittels Ultraschallsonotrode kontrolliert dispergiert wurden. Im Ergebnis wurde gezeigt, dass die Bestimmung der optimalen Ultraschallparameter möglich ist und die bis dahin übliche Praxis der experimentellen Bestimmung der Dispergierparameter für CNTs ablösen kann. Mithin wurde die Grundlage für die Herstellung elektrisch reproduzierbarer CNT-Polymer-Komposit-basierter Sensoren gelegt.
Darüber hinaus wurde das Anwendungspotential dieses Sensorkonzepts für Einzelsensoren zur punktuellen Druckmessung über eine Druckverteilungsmessung als Sensormatrix bis hin zur Anwendung als Einlegesohle im Schuh zur Überwachung des Drucks gezeigt. / Carbon nanotubes (CNT) polymer composites in the field of sensory applications have considerable potential. However, their electrical properties and their changes under mechanical stress play a decisive role. The deagglomeration process of the CNTs also has a great influence on the aspect ratio of the CNT agglomerates as well as the CNTs themselves and thus the electrical conductivity and reproducibility of the composite in both the mechanically unloaded and loaded state.This is shown by means of (partially) analytical models.
The dispersion quality is influenced by many factors. The process parameters during ultrasound dispersion are currently being determined by a trial-and-error method. Within the scope of the work, a dispersing equation for cylindrical particles, which are approximate to CNTs, was first developed, applied and verified for the dispersion of CNTs in solvents. The validity of the equation for CNTs was shown by the variation of the ultrasonic parameters time as well as energy and their influence on the degree of dispersion. The absorbance measured by means of UV-VIS spectroscopy serves as an indirect measure of the degree of dispersion. After pre-testing for suitable material selection, all relevant influencing parameters were calculated or determined experimentally. Experimental verification was carried out on CNT-N-methyl-2-pyrrolidone dispersions, which were dispersed in a controlled manner by means of an ultrasonic sonotrode.
As a result, it is illustrated that the determination of the optimal ultrasonic parameters is possible and can replace the conventional practice of the experimental determination of the dispersing parameters for CNTs. Accordingly, the basis for the production of electrically reproducible CNT polymer composite-based sensors has been established. In addition, the application potential of this sensor concept ranging from individual sensors for selective pressure measurement over pressure distribution measurement as a sensor matrix to the application as a shoe insole for pressure monitoring was shown.
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Generace kovových nanočástic v nízkoteplotním plazmatu v kapalině / Generation of metallic nanoparticles by non-thermal plasma in liquidsČechová, Ludmila January 2020 (has links)
This thesis focuses on the process of nanoparticle generation using new source of nonthermal plasma combining corona and pin-hole discharge in liquids. The theoretical part is focused on generation of metallic nanoparticles using various types of plasma discharge, the properties of metallic nanoparticles, their preparation by other methods and methods of characterization of nanoparticles. The experimental part deals with the preparation of copper, silver and gold nanoparticles from solutions of their precursors. The influence of experimental conditions, such as the influence of voltage polarity, effect of precursor concentration, effect of added electrolyte or reducing agent were investigated. All samples were analyzed by UV-VIS spectroscopy. Dynamic light scattering was used to determine the sice of nanoparticles. To confirm the presence of nanoparticles, samples were analyzed using scanning microscope with and energy dispersion spectrometer for elemental analysis.
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Využití chromatografie na tenké vrstvě k frakcionaci a charakterizaci organické hmoty izolované z alginitu / Use of thin layer chromatography for fractionation and characterization of organic matter isolated from alginiteSolanský, Pavel January 2021 (has links)
This diploma thesis is focused on the study of structure and physicochemical properties of organic fractions of humic substances, which were obtained by the method of thin-layer chromatography. Humic substances, which were used in this study, were isolated from a sample of Slovak alginite based on the procedure of the International Humic Substances Society (IHSS). The following analytical techniques were selected for the characterization of isolated humic substances: thermogravimetric and elemental analysis, molecular absorption spectroscopy (UV/Vis), Fourier transform infrared spectroscopy (FTIR) and steady-state fluorescence spectroscopy. Each organic fraction of humic substances were characterized by molecular absorption spectroscopy (UV/Vis) and steady-state fluorescence spectroscopy. Using steady-state fluorescence spectroscopy, humic substances were found to be composed of fluorophores of humic and non-humic (protein) character. Organic fractions corresponding to the humic fluorophores were characterized by a higher content of oxygen substituents on the aromatic nukleus, a higher degree of aromaticity and also a higher molecular weight. The aim of this diploma thesis was to design and optimize the process of organic matter fractionation for the purpose of detailed understanding of the structure and properties of humic substances, which were isolated from the sedimentary rock alginite. Based on this, the practical applicability of the thin layer chromatography method to significantly reduce the molecular heterogenity of the studied humic substances was evaluated.
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Srovnání plodů některých odrůd zimolezů z hlediska obsahu vybraných biologicky aktivních látek / Comparison of the fruits of some honeysuckle varieties in terms of content selected biologically active compoundsVeselý, Ondřej January 2015 (has links)
This thesis is focused to the analysis of selected varieties of honeysuckle kamtschatica (Lonicera caerula var kamtschatica) and their comparison in terms of the content of biologically active substances. There were analysed only varieties grown in 2014. Theoretical part elaborates and characterized various parameters of biologically active compounds such as phenolic, anthocyanins and ascorbic acid and possibilities of their determination. Further it briefly surveys Kamchatka honeysuckle, its taxonomic and morphological properties and its nutritional properties. The experimental part of the work was focused on the description of the methods used for the analysis of biologically active substances and their analysis. Polyphenolic compounds and anthocyanin’s were determined spectrophotometrically and vitamin C was determined by high-performance liquid chromatography. The results and varieties were compared with each other. Overall, we can say that the variety with the highest content of all three analysed biologically active substances is a variety Valchová, which had the second highest content of polyphenolic compounds (546.3 mg · 100 g-1 fruits), the third highest contend of ascorbic acid (35.1 mg · 100 g-1 fruits) and the sixth highest content of anthocyanin (170.8 mg · 100 g-1 fruits)
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