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- van Rhee, Frits (1)
- van Rheenen, Wouter (1)
- van Veen, Elke M. (1)
- van de Vlekkert, Diantha (1)
- van den Berg, Leonard H. (1)
- van den Hove, Daniel (1)
- van der Eerden, Bram C. J. (1)
- van der Linden, Mark (1)
- van der Spek, Rick A. (1)
- van der Werf, W. (1)
- von Collenberg, Cora R. (1)
- von Deimling, Andreas (1)
- von Eyss, Björn (1)
- von Gontard, Alexander (1)
- von Kalle, Thekla (1)
- von Kistowski, Jóakim Gunnarsson (1)
- Álmos, Péter Z. (1)
- Üceyler, Nurcan (1)
- Ülzen, Anett (1)
Institute
- Theodor-Boveri-Institut für Biowissenschaften (97)
- Graduate School of Life Sciences (51)
- Physikalisches Institut (44)
- Medizinische Klinik und Poliklinik II (33)
- Institut für Psychologie (32)
- Institut für Anorganische Chemie (27)
- Institut für Organische Chemie (27)
- Neurologische Klinik und Poliklinik (27)
- Rudolf-Virchow-Zentrum (23)
- Abteilung für Funktionswerkstoffe der Medizin und der Zahnheilkunde (20)
Schriftenreihe
Sonstige beteiligte Institutionen
- Johns Hopkins School of Medicine (2)
- VolkswagenStiftung (2)
- Bio-Imaging Center Würzburg (1)
- CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - the development agency of the Brazilian Federal Government (1)
- Center for Nanosystems Chemistry (CNC), Universität Würzburg (1)
- DAAD - Deutscher Akademischer Austauschdienst (1)
- Department of Hematology and Oncology, Sana Hospital Hof, Hof, Germany (1)
- Department of Laboratory Medicine and Medicine Huddinge, Karolinska Institutet and University Hospital, Stockholm, Sweden (1)
- Department of Medicine A, University Hospital of Münster, Münster, Germany (1)
- Ernst Strüngmann Institute for Neuroscience in Cooperation with Max Planck Society (ESI) (1)
ResearcherID
- B-4606-2017 (1)
The FDA approval of targeted therapy with BRAFV600E inhibitors like vemurafenib and dabrafenib in 2011 has been the first major breakthrough in the treatment of metastatic melanoma since almost three decades. Despite increased progression free survival and elevated overall survival rates, complete responses are scarce due to resistance development approximately six months after the initial drug treatment. It was previously shown in our group that melanoma cells under vemurafenib pressure in vitro and in vivo exhibit features of drug-induced senescence. It is known that some cell types, which undergo this cell cycle arrest, develop a so-called senescence associated secretome and it has been reported that melanoma cell lines also upregulate the expression of different factors after senescence induction. This work describes the effect of the vemurafenib-induced secretome on cells. Conditioned supernatants of vemurafenib-treated cells increased the viability of naive fibroblast and melanoma cell lines. RNA analysis of donor melanoma cells revealed elevated transcriptional levels of FGF1, MMP2 and CCL2 in the majority of tested cell lines under vemurafenib pressure, and I could confirm the secretion of functional proteins. Similar observations were also done after MEK inhibition as well as in a combined BRAF and MEK inhibitor treatment situation. Interestingly, the transcription of other FGF ligands (FGF7, FGF17) was also elevated after MEK/ERK1/2 inhibition. As FGF receptors are therapeutically relevant, I focused on the analysis of FGFR-dependent processes in response to BRAF inhibition. Recombinant FGF1 increased the survival rate of melanoma cells under vemurafenib pressure, while inhibition of the FGFR pathway diminished the viability of melanoma cells in combination with vemurafenib and blocked the stimulatory effect of vemurafenib conditioned medium. The BRAF inhibitor induced secretome is regulated by active PI3K/AKT signaling, and the joint inhibition of mTor and BRAFV600E led to decreased senescence induction and to a diminished induction of the secretome-associated genes. In parallel, combined inhibition of MEK and PI3K also drastically decreased mRNA levels of the relevant secretome components back to basal levels.
In summary, I could demonstrate that BRAF inhibitor treated melanoma cell lines acquire a specific PI3K/AKT dependent secretome, which is characterized by FGF1, CCL2 and MMP2. This secretome is able to stimulate other cells such as naive melanoma cells and fibroblasts and contributes to a better survival under drug pressure. These data are therapeutically highly relevant, as they imply the usage of novel drug combinations, especially specific FGFR inhibitors, with BRAF inhibitors in the clinic.
Surface systems attract great scientific attention due to novel and exotic properties. The atomically structured surfaces lead to a reduced dimensionality which alters electronic correlations, vibrational properties, and their impact on each other. The emerging physical phenomena are not observed for related bulk materials. In this thesis, ordered (sub)monolayers of metal atoms (Au and Sn) on semiconductor substrates (Si(111) and Ge(111)) and ultrathin intermetallic films (CePt5 and LaPt5) on metal substrate (Pt(111)) are investigated by polarized in situ surface Raman spectroscopy. The surface Raman spectra exhibit features of specific elementary excitations like surface phonons and electronic excitations, which are suitable to gain fundamental insights into the surface systems.
The Au-induced surface reconstructions (5x2) and (r3xr3) constitute quasi-one- and two-dimensional Au structures on the Si(111) substrate, respectively. The new reconstruction-related Raman peaks are analyzed with respect to their polarization and temperature behavior. The Raman results are combined with firstprinciples calculations to decide between different proposed structural models. The Au-(5x2)/Si(111) reconstruction is best described by the model of Kwon and Kang, while for Au-(r3xr3)/Si(111) the conjugate honeycomb-chained-trimer model is favored. The Sn-induced reconstructions with 1/3 monolayer on Ge(111) and Si(111) are investigated to reveal their extraordinary temperature behavior. Specific surface phonon modes are identified that are predicted within the dynamical fluctuation model. Contrary to Sn/Si(111), the corresponding vibrational mode of Sn/Ge(111) exhibits a nearly harmonic character. The reversible structural phase transition of Sn/Ge(111) from (r3xr3) to (3x3) is observed, while no phase transition is apparent for Sn/Si(111). Moreover, Raman spectra of the closely related systems Sn-(2r3x2r3)/Si(111) and thin films of a-Sn as well as the clean semiconductor surfaces Si(111)-(7x7) and Ge(111)-c(2x8) are evaluated and compared.
The CePt5/Pt(111) system hosts 4f electrons whose energy levels are modified by the crystal field and are relevant for a description of the observed Kondo physics. In contrast, isostructural LaPt5/Pt(111) has no 4f electrons. For CePt5/Pt(111), distinct Raman features due to electronic Raman scattering can be unambiguously related to transitions between the crystal-field states which are depth-dependent. This assignment is supported by comparison to LaPt5/Pt(111) and group theoretical considerations. Furthermore, the vibrational properties of CePt5 and LaPt5 reveal interesting similarities but also striking differences like an unusual temperature shift of a vibration mode of CePt5, which is related to the influence of 4f electrons.
Automation in Software Performance Engineering Based on a Declarative Specification of Concerns
(2019)
Software performance is of particular relevance to software system design, operation, and evolution because it has a significant impact on key business indicators. During the life-cycle of a software system, its implementation, configuration, and deployment are subject to multiple changes that may affect the end-to-end performance characteristics. Consequently, performance analysts continually need to provide answers to and act based on performance-relevant concerns. To ensure a desired level of performance, software performance engineering provides a plethora of methods, techniques, and tools for measuring, modeling, and evaluating performance properties of software systems. However, the answering of performance concerns is subject to a significant semantic gap between the level on which performance concerns are formulated and the technical level on which performance evaluations are actually conducted. Performance evaluation approaches come with different strengths and limitations concerning, for example, accuracy, time-to-result, or system overhead. For the involved stakeholders, it can be an elaborate process to reasonably select, parameterize and correctly apply performance evaluation approaches, and to filter and interpret the obtained results. An additional challenge is that available performance evaluation artifacts may change over time, which requires to switch between different measurement-based and model-based performance evaluation approaches during the system evolution. At model-based analysis, the effort involved in creating performance models can also outweigh their benefits.
To overcome the deficiencies and enable an automatic and holistic evaluation of performance throughout the software engineering life-cycle requires an approach that: (i) integrates multiple types of performance concerns and evaluation approaches, (ii) automates performance model creation, and (iii) automatically selects an evaluation methodology tailored to a specific scenario. This thesis presents a declarative approach —called Declarative Performance Engineering (DPE)— to automate performance evaluation based on a humanreadable specification of performance-related concerns. To this end, we separate the definition of performance concerns from their solution. The primary scientific contributions presented in this thesis are:
A declarative language to express performance-related concerns and a corresponding processing framework:
We provide a language to specify performance concerns independent of a concrete performance evaluation approach. Besides the specification of functional aspects, the language allows to include non-functional tradeoffs optionally. To answer these concerns, we provide a framework architecture and a corresponding reference implementation to process performance concerns automatically. It allows to integrate arbitrary performance evaluation approaches and is accompanied by reference implementations for model-based and measurement-based performance evaluation.
Automated creation of architectural performance models from execution traces:
The creation of performance models can be subject to significant efforts outweighing the benefits of model-based performance evaluation. We provide a model extraction framework that creates architectural performance models based on execution traces, provided by monitoring tools.The framework separates the derivation of generic information from model creation routines. To derive generic information, the framework combines state-of-the-art extraction and estimation techniques. We isolate object creation routines specified in a generic model builder interface based on concepts present in multiple performance-annotated architectural modeling formalisms. To create model extraction for a novel performance modeling formalism, developers only need to write object creation routines instead of creating model extraction software from scratch when reusing the generic framework.
Automated and extensible decision support for performance evaluation approaches:
We present a methodology and tooling for the automated selection of a performance evaluation approach tailored to the user concerns and application scenario. To this end, we propose to decouple the complexity of selecting a performance evaluation approach for a given scenario by providing solution approach capability models and a generic decision engine. The proposed capability meta-model enables to describe functional and non-functional capabilities of performance evaluation approaches and tools at different granularities. In contrast to existing tree-based decision support mechanisms, the decoupling approach allows to easily update characteristics of solution approaches as well as appending new rating criteria and thereby stay abreast of evolution in performance evaluation tooling and system technologies.
Time-to-result estimation for model-based performance prediction:
The time required to execute a model-based analysis plays an important role in different decision processes. For example, evaluation scenarios might require the prediction results to be available in a limited period of time such that the system can be adapted in time to ensure the desired quality of service. We propose a method to estimate the time-to-result for modelbased performance prediction based on model characteristics and analysis parametrization. We learn a prediction model using performancerelevant features thatwe determined using statistical tests. We implement the approach and demonstrate its practicability by applying it to analyze a simulation-based multi-step performance evaluation approach for a representative architectural performance modeling formalism.
We validate each of the contributions based on representative case studies. The evaluation of automatic performance model extraction for two case study systems shows that the resulting models can accurately predict the performance behavior. Prediction accuracy errors are below 3% for resource utilization and mostly less than 20% for service response time. The separate evaluation of the reusability shows that the presented approach lowers the implementation efforts for automated model extraction tools by up to 91%. Based on two case studies applying measurement-based and model-based performance evaluation techniques, we demonstrate the suitability of the declarative performance engineering framework to answer multiple kinds of performance concerns customized to non-functional goals. Subsequently, we discuss reduced efforts in applying performance analyses using the integrated and automated declarative approach. Also, the evaluation of the declarative framework reviews benefits and savings integrating performance evaluation approaches into the declarative performance engineering framework. We demonstrate the applicability of the decision framework for performance evaluation approaches by applying it to depict existing decision trees. Then, we show how we can quickly adapt to the evolution of performance evaluation methods which is challenging for static tree-based decision support systems. At this, we show how to cope with the evolution of functional and non-functional capabilities of performance evaluation software and explain how to integrate new approaches. Finally, we evaluate the accuracy of the time-to-result estimation for a set of machinelearning algorithms and different training datasets. The predictions exhibit a mean percentage error below 20%, which can be further improved by including performance evaluations of the considered model into the training data. The presented contributions represent a significant step towards an integrated performance engineering process that combines the strengths of model-based and measurement-based performance evaluation. The proposed performance concern language in conjunction with the processing framework significantly reduces the complexity of applying performance evaluations for all stakeholders. Thereby it enables performance awareness throughout the software engineering life-cycle. The proposed performance concern language removes the semantic gap between the level on which performance concerns are formulated and the technical level on which performance evaluations are actually conducted by the user.
The plasma membrane is one of the most thoroughly studied and at the same time most complex, diverse, and least understood cellular structures. Its function is determined by the molecular composition as well as the spatial arrangement of its components. Even after decades of extensive membrane research and the proposal of dozens of models and theories, the structural organization of plasma membranes remains largely unknown. Modern imaging tools such as super-resolution fluorescence microscopy are one of the most efficient techniques in life sciences and are widely used to study the spatial arrangement and quantitative behavior of biomolecules in fixed and living cells. In this work, direct stochastic optical reconstruction microscopy (dSTORM) was used to investigate the structural distribution of mem-brane components with virtually molecular resolution. Key issues are different preparation and staining strategies for membrane imaging as well as localization-based quantitative analyses of membrane molecules.
An essential precondition for the spatial and quantitative analysis of membrane components is the prevention of photoswitching artifacts in reconstructed localization microscopy images. Therefore, the impact of irradiation intensity, label density and photoswitching behavior on the distribution of plasma membrane and mitochondrial membrane proteins in dSTORM images was investigated. It is demonstrated that the combination of densely labeled plasma membranes and inappropriate photoswitching rates induces artificial membrane clusters. Moreover, inhomogeneous localization distributions induced by projections of three-dimensional membrane structures such as microvilli and vesicles are prone to generate artifacts in images of biological membranes. Alternative imaging techniques and ways to prevent artifacts in single-molecule localization microscopy are presented and extensively discussed.
Another central topic addresses the spatial organization of glycosylated components covering the cell membrane. It is shown that a bioorthogonal chemical reporter system consisting of modified monosaccharide precursors and organic fluorophores can be used for specific labeling of membrane-associated glycoproteins and –lipids. The distribution of glycans was visualized by dSTORM showing a homogeneous molecule distribution on different mammalian cell lines without the presence of clusters. An absolute number of around five million glycans per cell was estimated and the results show that the combination of metabolic labeling, click chemistry, and single-molecule localization microscopy can be efficiently used to study cell surface glycoconjugates.
In a third project, dSTORM was performed to investigate low-expressing receptors on cancer cells which can act as targets in personalized immunotherapy. Primary multiple myeloma cells derived from the bone marrow of several patients were analyzed for CD19 expression as potential target for chimeric antigen receptor (CAR)-modified T cells. Depending on the patient, 60–1,600 CD19 molecules per cell were quantified and functional in vitro tests demonstrate that the threshold for CD19 CAR T recognition is below 100 CD19 molecules per target cell. Results are compared with flow cytometry data, and the important roles of efficient labeling and appropriate control experiments are discussed.
Neuroimaging research has highlighted the relevance of well-balanced functional brain interactions as an essential basis for efficient emotion regulation. In contrast, abnormal coupling of fear-processing regions such as the amygdala, the anterior cingulate cortex (ACC) and the insula could be an important feature of anxiety disorders. Although activity alterations of these regions have been frequently reported in specific phobia, little is known about their functional interactions during phobogenic stimulus processing.
To explore these interrelationships in two subtypes of specific phobia – i.e., the blood-injection-injury subtype and the animal subtype – functional connectivity (FC) was analyzed in three fMRI studies. Two studies examined fear processing in a dental phobia group (DP), a snake phobia group (SP) and a healthy control group (HC) during visual phobogenic stimuli presentation while a third study investigated differences between auditory and visual stimuli presentation in DP and HC.
Due to a priori hypotheses of impaired interactions between the amygdala, the ACC and the insula, a first analysis was conducted to explore the FC within these three regions of interest. Based on emerging evidence of functionally diverse subregions, the ACC was further divided into a subgenual, pregenual and dorsal ACC and the insula was divided into a ventral-anterior, dorsal-anterior and posterior region. Additionally, an exploratory seed-to-voxel analysis using the amygdala, ACC and insula as seeds was conducted to scan for connectivity patterns across the whole brain.
The analyses revealed a negative connectivity of the ACC and the amygdala during phobogenic stimulus processing in controls. This connectivity was predominantly driven by the affective ACC subdivision. By contrast, SP was characterized by an increased mean FC between the examined regions. Interestingly, this phenomenon was specific for auditory, but not visual symptom provocation in DP. During visual stimulus presentation, however, DP exhibited further FC alterations of the ACC and the insula with pre- and orbitofrontal regions.
These findings mark the importance of balanced interactions between fear-processing regions in specific phobia, particularly of the inhibitory connectivity between the ACC and the amygdala. Theoretically, this is assumed to reflect top-down inhibition by the ACC during emotion regulation. The findings support the suggestion that SP particularly is characterized by excitatory, or missing inhibitory, (para-) limbic connectivity, reflecting an overshooting fear response based on evolutionary conserved autonomic bottom-up pathways. Some of these characteristics applied to DP as well but only under the auditory stimulation, pointing to stimulus dependency. DP was further marked by altered pre- and orbitofrontal coupling with the ACC and the insula which might represent disturbances of superordinate cognitive control on basal emotion processes. These observations strengthen the assumption that DP is predominantly based on evaluation-based fear responses.
In conclusion, the connectivity patterns found may depict an intermediate phenotype that possibly confers risks for inappropriate phobic fear responses. The findings presented could also be of clinical interest. Particularly the ACC – amygdala circuit may be used as a predictive biomarker for treatment response or as a promising target for neuroscience-focused augmentation strategies as neurofeedback or repetitive transcranial magnetic stimulation.
Upon approval of a drug, the stability of the API and the FPP has to be studied intensively because it determines the shelf-life. If a drug is found to be stable, the expiry date is arbitrary set to five years at the maximum, if a drug tends to undergo degradation, the expiry date is set shorter. The drug product must comply with predefined specifications in accordance with the ICH guidelines Q6A and Q6B during its entire market life. The content of the active substance is required to be within a specification of 95–105% of its labeled claim until expiry corresponding to the ICH guideline Q1A(R2). However, there is little or scattered literature information addressing the stability of drug products beyond their expiry dates. The objective of this thesis was to study and assess the long-term stability of a collection involving numerous pure drug substances and ampoules manufactured in the 20th century. The content and the impurity profile were examined by means of appropriate analytical methods, mainly using liquid chromatography. The results were compared to data being available in the literature. Assessing the stability regarding the dosage form and the affiliation of the drug class was conducted.
The experimental studies comprise the examination of 50 drug substances manufactured 20–30 years ago and 14 long expired ampoules which were older than 40 years in the time of analysis, exceeding many times the maximum shelf life of five years.
For investigation of the solid drug substances, pharmacopoeial methods were applied as far as possible. Indeed, results of the study showed that 44 tested substances still complied with the specification of the Ph. Eur. with regard to the content and impurity profile, even after more than two decades of storage.
For analysis of the injection solutions, HPLC-UV and HPLC-ESI/MS techniques were applied, commonly based on liquid chromatography methods of the Ph. Eur. for determination of related substances. Each method was further validated for its application to ensure accurate API quantification corresponding to ICH Q2(R1). Quite a few ampoules were identified to show surprisingly high stability. In spite of their age of 53–72 years, APIs such as caffeine, etilefrine, synephrine, metamizole sodium, furosemide, and sodium salicylate complied with the specified content that is valid nowadays, respectively. Nevertheless, typical degradation reaction, e.g. hydrolysis, oxidation, or isomerization, was observed in all remaining ampoules. Various degrees of hydrolysis were revealed for scopolamine, procaine, and adenosine triphosphate, the contents were decreased to 71%, 70%, and 15% of the declared concentrations, respectively. In the epinephrine and dipyridamole ampoules, oxidative degradation has been occurred, finding respective API contents of more or less 70%. For dihydroergotamine, excessive decomposition by epimerization was observed, resulting in an API content of 21% and degradation by isomerization was found in lobeline, still containing 64% of the labeled claim.
In conclusion, supported by the data of the present studies and the literature, defining and authorizing a longer shelf-life may be applicable to numerous pharmaceuticals which should be considered by pharmaceutical manufacturers and regulatory authorities, if justified based on stability studies. A general extension of the shelf-lives of drug products and the abolishment or extension of the maximum shelf-life limit of five years would prevent disposing of still potent medications and save a lot of money to the entire health care system.
Introduction: Speckle-tracking echocardiography has recently emerged as a quantitative ultrasound technique for accurately evaluating myocardial function by analyzing the motion of speckles identified. Speckle-tracking obtained under stress may offer an opportunity to improve the detection of dynamic regional abnormalities and myocardial viability.
Objective: To evaluate stress speckle tracking as tool to detect myocardial viability in comparison to cardiac MRI in post-STEMI patients.
Methods: 49 patients were prospectively enrolled in our 18-month’s study. Dobutamin stress echocardiography was performed 4 days post-infarction accompanied with automated functional imaging (Speckle tracking) analysis of left ventricle during rest and then during low dose stress. All patients underwent a follow up stress echocardiography at 6 weeks with speckle tracking analysis. Cardiac MRI took place concomitantly at 4 days post-infarction and 6 weeks. We carried out an assessment of re-admission with acute coronary syndrome (ACS) after one year of enrollment.
Results: Investigating strain rate obtained with stress speckle tracking after revascularization predicted the extent of myocardial scar, determined by contrast-enhanced magnetic resonance imaging. A good correlation was found between the global strain and total infarct size (R 0.75, p< 0.001). Furthermore, a clear inverse relationship was found between the segmental strain and the transmural extent of infarction in each segment. (R -0.69, p<0.01). Meanwhile it provided 81.82% sensitivity and 82.6% specificity to detect transmural from non-transmural infarction at a cut-off value of -10.15. Global stress strain rate showed 80% sensitivity and 77.5% specificity at a cut-off value of -9.1 to predict hospital re-admission with ACS. A cut-off value of -8.4 had shown a 69.23% sensitivity and 73.5% specificity to predict the re-admission related to other cardiac symptoms.
Conclusion: Strain rate obtained from speckle tracking during stress is a novel method of detecting myocardial viability after STEMI .Moreover it carries a promising role in post-myocardial infarction risk stratification with a reasonable prediction of reversible cardiac-related hospital re-admission.
Motivated by the great potential which is offered by the combination of additive manufacturing and tissue engineering, a novel polymeric bioink platform based on poly(2 oxazoline)s was developed which might help to further advance the young and upcoming field of biofabrication. In the present thesis, the synthesis as well as the characteristics of several diblock copolymers consisting of POx and POzi have been investigated with a special focus on their suitability as bioinks.
In general, the copolymerization of 2-oxazolines and 2-oxazines bearing different alkyl side chains was demonstrated to yield polymers in good agreement with the degree of polymerization aimed for and moderate to low dispersities.
For every diblock copolymer synthesized during the present study, a more or less pronounced dependency of the dynamic viscosity on temperature could be demonstrated. Diblock copolymers comprising a hydrophilic PMeOx block and a thermoresponsive PnPrOzi block showed temperature induced gelation above a degree of polymerization of 50 and a polymer concentration of 20 wt%. Such a behavior has never been described before for copolymers solely consisting of poly(cyclic imino ether)s.
Physically cross linked hydrogels based on POx b POzi copolymers exhibit reverse thermal gelation properties like described for solutions of PNiPAAm and Pluronic F127. However, by applying SANS, DLS, and SLS it could be demonstrated that the underlying gel formation mechanism is different for POx b POzi based hydrogels. It appears that polymersomes with low polydispersity are formed already at very low polymer concentrations of 6 mg/L. Increasing the polymer concentration resulted in the formation of a bicontinuous sponge like structure which might be formed due to the merger of several vesicles. For longer polymer chains a phase transition into a gyroid structure was postulated and corresponds well with the observed rheological data.
Stable hydrogels with an unusually high mechanical strength (G’ ~ 4 kPa) have been formed above TGel which could be adjusted over a range of 20 °C by changing the degree of polymerization if maintaining the symmetric polymer architecture. Variations of the chain ends revealed only a minor influence on TGel whereas the influence of the solvent should not be neglected as shown by a comparison of cell culture medium and MilliQ water.
Rotationally as well as oscillatory rheological measurements revealed a high suitability for printing as POx b POzi based hydrogels exhibit strong shear thinning behavior in combination with outstanding recovery properties after high shear stress.
Cell viability assays (WST-1) of PMeOx b PnPrOzi copolymers against NIH 3T3 fibroblasts and HaCat cells indicated that the polymers were well tolerated by the cells as no dose-dependent cytotoxicity could be observed after 24 h at non-gelling concentrations up to 100 g/L.
In summary, copolymers consisting of POx and POzi significantly increased the accessible range of properties of POx based materials. In particular thermogelation of aqueous solutions of diblock copolymers comprising PMeOx and PnPrOzi was never described before for any copolymer consisting solely of POx or POzi. In combination with other characteristics, e.g. very good cytocompatibility at high polymer concentrations and comparably high mechanical strength, the formed hydrogels could be successfully used for 3D bioprinting. Although the results appear promising and the developed hydrogel is a serious bioink candidate, competition is tough and it remains an open question which system or systems will be used in the future.
Stennett, Tom E. ; Bissinger, Philipp ; Griesbeck, Stefanie ; Ullrich, Stefan ; Krummenacher, Ivo ; Auth, Michael ; Sperlich, Andreas ; Stolte, Matthias ; Radacki, Krzysztof ; Yao, Chang-Jiang ; Würthner, Frank ; Steffen, Andreas ; Marder, Todd B. ; Braunschweig, Holger
In this work, two new quadrupolar A-π-D-π-A chromophores have been prepared featuring a strongly electron- donating diborene core and strongly electron-accepting dimesitylboryl F(BMes2) and bis(2,4,6-tris(trifluoromethyl)phenyl)boryl (BMes2) end groups. Analysis of the compounds by NMR spectroscopy, X-ray crystallography, cyclic voltammetry and UV-vis-NIR absorption and emission spectroscopy indicated that the compounds possess extended conjugated π-systems spanning their B4C8 cores. The combination of exceptionally potent π-donor (diborene) and π- acceptor (diarylboryl) groups, both based on trigonal boron, leads to very small HOMO-LUMO gaps, resulting in strong absorption in the near-IR region with maxima in THF at 840 and 1092 nm, respectively, and very high extinction coefficients of ca. 120,000 M-1cm-1. Both molecules also display weak near-IR fluorescence with small Stokes shifts.
In this thesis, the photophysics and spin chemistry of donor-photosensitizer-acceptor triads were investigated. While all investigated triads comprised a TAA as an electron donor and a NDI as an electron acceptor, the central photosensitizers (PS) were different chromophores based on the dipyrrin-motif. The purity and identity of all target compounds could be confirmed by NMR spectroscopy, mass spectrometry and elemental analysis.
The first part of the work dealt with dipyrrinato-complexes of cyclometalated heavy transition metals. The successful synthesis of novel triads based on Ir(III), Pt(II) and Pd(II) was presented. The optical and electrochemical properties indicated charge separation (CS), which was confirmed by transient absorption (TA) spectroscopy. TA-spectroscopy also revealed that the process of CS is significantly slower and less efficient for the triads based on Pt(II) and Pd(II) than for the analogous Ir(III) triads. This is mostly due to a much more convoluted reaction pathway, comprising several intermediate states before the formation of the final charge separated state (CSS2). On the other hand, CSS2 exhibits long lifetimes which are dependent on the central metal ion. While the Ir(III) triads show lifetimes of about 0.5 µs in MeCN, the Pt(II) and Pd(II) analogues show lifetimes of 1.5 µs. The magnetic field effect on the charge recombination (CR) kinetics of CSS2 was investigated by magnetic field dependent ns-TA spectroscopy and could be rationalized based on a classical kinetic scheme comprising only one magnetic field dependent rate constant k±. The behavior of k± shows a clear separation of the coherent and incoherent spin interconversion mechanisms. While the coherent spin evolution is due to the isotropic hyperfine coupling with the magnetic nuclei of the radical centers, the incoherent spin relaxation is due to a rotational modulation of the anisotropic hyperfine coupling tensor and is strongly dependent on the viscosity of the solvent. This dependence could be used to measure the nanoviscosity of the oligomeric solvent pTHF, which was found to be distinctly different from its macroviscosity.
The second part of the work dealt with bisdipyrrinato complexes and their bridged porphodimethenato (PDM) analogues. Initially, the suitability of the different chromophores for the use as PS in donor-acceptor substituted triads was tested by a systematic investigation of their steady state and transient properties. While the PDM-complex of Zn(II) and Pd(II) exhibited promising characteristics such as a high exited state lifetime and relatively intense emission, the purely organic parent PDM and the non-bridged bisdipyrrinato-Pd(II) complex were less suitable. The difference between the two Pd(II) complexes could be explained by a structural rearrangement of the non-bridged complex which results in a non-emissive metal centered triplet state with disphenoidal geometry. This rearrangement is prevented by the dimethylmethylene-bridges in the bridged analogue resulting in higher phosphorescence quantum yields and excited state lifetimes.
With the exception of the Zn(II)PDM-complex, the synthesis of novel donor acceptor substituted triads could be realized for all desired central chromophores. They were investigated equivalently to the cyclometalated triads described in the first part. The steady state properties indicate a stronger electronic coupling between the subunits due to the lack of unsaturated bridges between the donor and the central chromophore. Photoinduced CS occurs in all investigated triads. Due to the low exited state lifetimes of the central chromophores, CSS is formed less efficiently for the triads based on the unbridged Pd(II)-complex as well as the purely organic PDM. In the triad based on the bridged Pd(II) complex, the CR of CSS2 is faster than its formation resulting in low intermediate concentrations. For its elongated analogue, this is not the case and CSS2 can be observed clearly. Although the spin-chemistry of the triads based on bisdipyrrinato-Pd(II) and porphodimethenato-Pd(II) is less well understood, first interpretations of the magnetic field dependent decay kinetics gave results approximately equivalent to those obtained for the cyclometalated triads. Furthermore, the MFE was shown to be useful for the investigation of the quantum yield of CS and the identity of the observed CSSs.
In both parts of this work, the influence of the central photosensitizer on the photophysics and the spin chemistry of the triads could be shown. While the process of CS is directly dependent on the PS, the PS usually is not directly involved in the final CSSs. None the less, it can still indirectly affect the CR and spin chemistry of the CSS since it influences the electronic coupling between donor and acceptor, as well as the geometry of the triads.