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    Surface cleaning and sample carrier for complementary high-resolution imaging techniques
    (Melville, NY : AIP, 2020) Benettoni, Pietro; Ye, Jia-Yu; Holbrook, Timothy R.; Calabrese, Federica; Wagner, Stephan; Zarejousheghani, Mashaalah; Griebe, Jan; Ullrich, Maria K.; Musat, Niculina; Schmidt, Matthias; Flyunt, Roman; Reemtsma, Thorsten; Richnow, Hans-Hermann; Stryhanyuk, Hryhoriy
    Nowadays, high-resolution imaging techniques are extensively applied in a complementary way to gain insights into complex phenomena. For a truly complementary analytical approach, a common sample carrier is required that is suitable for the different preparation methods necessary for each analytical technique. This sample carrier should be capable of accommodating diverse analytes and maintaining their pristine composition and arrangement during deposition and preparation. In this work, a new type of sample carrier consisting of a silicon wafer with a hydrophilic polymer coating was developed. The robustness of the polymer coating toward solvents was strengthened by cross-linking and stoving. Furthermore, a new method of UV-ozone cleaning was developed that enhances the adhesion of the polymer coating to the wafer and ensures reproducible surface-properties of the resulting sample carrier. The hydrophilicity of the sample carrier was recovered applying the new method of UV-ozone cleaning, while avoiding UV-induced damages to the polymer. Noncontact 3D optical profilometry and contact angle measurements were used to monitor the hydrophilicity of the coating. The hydrophilicity of the polymer coating ensures its spongelike behavior so that upon the deposition of an analyte suspension, the solvent and solutes are separated from the analyte by absorption into the polymer. This feature is essential to limit the coffee-ring effect and preserve the native identity of an analyte upon deposition. The suitability of the sample carrier for various sample types was tested using nanoparticles from suspension, bacterial cells, and tissue sections. To assess the homogeneity of the analyte distribution and preservation of sample integrity, optical and scanning electron microscopy, helium ion microscopy, laser ablation inductively coupled plasma mass spectrometry, and time-of-flight secondary ion mass spectrometry were used. This demonstrates the broad applicability of the newly developed sample carrier and its value for complementary imaging. © 2020 Author(s).
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    Estradiol Removal by Adsorptive Coating of a Microfiltration Membrane
    (Basel : MDPI, 2021) Niavarani, Zahra; Breite, Daniel; Prager, Andrea; Abel, Bernd; Schulze, Agnes
    This work demonstrates the enhancement of the adsorption properties of polyethersulfone (PES) microfiltration membranes for 17β-estradiol (E2) from water. This compound represents a highly potent endocrine-disrupting chemical (EDC). The PES membranes were modified with a hydrophilic coating functionalized by amide groups. The modification was performed by the interfacial reaction between hexamethylenediamine (HMD) or piperazine (PIP) as the amine monomer and trimesoyl chloride (TMC) or adipoyl chloride (ADC) as the acid monomer on the surface of the membrane using electron beam irradiation. The modified membranes and the untreated PES membrane were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), water permeance measurements, water contact angle measurements, and adsorption experiments. Furthermore, the effects of simultaneous changes in four modification parameters: amine monomer types (HMD or PIP), acid monomer types (TMC or ADC), irradiation dosage (150 or 200 kGy), and the addition of toluene as a swelling agent, on the E2 adsorption capacity were investigated. The results showed that the adsorption capacities of modified PES membranes toward E2 are >60%, while the unmodified PES membrane had an adsorption capacity up to 30% for E2 under similar experimental conditions, i.e., an enhancement of a factor of 2. Next to the superior adsorption properties, the modified PES membranes maintain high water permeability and no pore blockage was observed. The highlighted results pave the way to develop efficient low-cost, stable, and high-performance adsorber membranes.
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    In situ Gelling Amphotericin B Nanofibers: A New Option for the Treatment of Keratomycosis
    (Lausanne : Frontiers Media, 2020) Göttel, Benedikt; Lucas, Henrike; Syrowatka, Frank; Knolle, Wolfgang; Kuntsche, Judith; Heinzelmann, Joana; Viestenz, Arne; Mäder, Karsten
    The purpose of our research was the development of Amphotericin B-loaded in situ gelling nanofibers for the treatment of keratomycosis. Different formulation strategies were applied to increase the drug load of the sparingly water-soluble Amphotericin B in electrospun Gellan Gum/Pullulan fibers. These include bile salt addition, encapsulation in poly(lactic-co-glycolic acid) (PLGA) nanoparticles and formation of a polymeric Amphotericin B polyelectrolyte complex. The Amphotericin B polyelectrolyte complex (AmpB-Eu L) performed best and was very effective against the fungal strain Issatchenkia orientalis in vitro. The complex was characterized in detail by attenuated total reflection infrared spectroscopy, X-ray powder diffraction, and differential scanning calorimetry. A heat induced stress test was carried out to ensure the stability of the polyelectrolyte complex. To gain information about the cellular tolerance of the developed polyelectrolyte complex a new, innovative multilayered-stratified human cornea cell model was used for determination of the cellular toxicity in vitro. For a safe therapy, the applied ophthalmic drug delivery system has to be sterile. Sterilization by electron irradiation caused not degradation of pure Amphotericin B and also for the bile salt complex. Furthermore, the developed Amphotericin B polyelectrolyte complex was not degraded by the irradiation process. In conclusion, a new polyelectrolyte Amphotericin B complex has been found which retains the antifungal activity of the drug with sufficient stability against irradiation-sterilization induced drug degradation. Furthermore, in comparison with the conventional used eye drop formulation, the new AmpB-complex loaded nanofibers were less toxic to cornea cells in vitro. Electrospinning of the Amphotericin B polyelectrolyte complex with Gellan Gum/ Pullulan leads to the formation of nanofibers with in situ gelling properties, which is a new and promising option for the treatment of keratomycosis. © Copyright © 2020 Göttel, Lucas, Syrowatka, Knolle, Kuntsche, Heinzelmann, Viestenz and Mäder.
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    Regeneration of TiO 2 Nanotube Arrays after Long-Term Cell and Tissue Culture for Multiple Use - An Environmental Scanning Electron Microscopy (ESEM) Survey of Adult Pig Retina and beyond
    (New York, NY : Springer, 2019) Friebe, Sabrina; Mayr, Stefan G.
    Long-term organotypic culture of adult tissues not only open up possibilities for studying complex structures of explants in vitro, but also can be employed e.g. to investigate pathological changes, their fingerprints on tissue mechanics, as well as the effectiveness of drugs. While conventional culture methods do not allow for survival times of more than a few days, we have demonstrated recently that TiO 2 nanotube arrays allow to maintain integrity of numerous tissues, including retina, brain, spline and tonsils, for as long as 2 weeks in vitro. A mystery in culturing has been the interaction of tissue with these substrates, which is also reflected by tissue debris after liftoff. As the latter reveals fingerprints of tissue adhesion and impedes with nanotube array reuse, we address within the present environmental scanning electron study debris nature and the effectiveness of cleaning approaches of distinct physical and chemical methods, including UV-light irradiation, O2 plasma treatment and application of an enzyme-based buffer. This will lays the foundation for large-scale regeneration and reuse of nanotube arrays in science and clinical research. © 2019 The Author(s).
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    Curvature model for nanoparticle size effects on peptide fibril stability and molecular dynamics simulation data
    (Amsterdam [u.a.] : Elsevier, 2022) John, Torsten; Martin, Lisandra L.; Risselada, Herre Jelger; Abel, Bernd
    Nanostructured surfaces are widespread in nature and are being further developed in materials science. This makes them highly relevant for biomolecules, such as peptides. In this data article, we present a curvature model and molecular dynamics (MD) simulation data on the influence of nanoparticle size on the stability of amyloid peptide fibrils related to our research article entitled “Mechanistic insights into the size-dependent effects of nanoparticles on inhibiting and accelerating amyloid fibril formation” (John et al., 2022) [1]. We provide the code to perform MD simulations in GROMACS 4.5.7 software of arbitrarily chosen biomolecule oligomers adsorbed on a curved surface of chosen nanoparticle size. We also provide the simulation parameters and data for peptide oligomers of Aß40, NNFGAIL, GNNQQNY, and VQIYVK. The data provided allows researchers to further analyze our MD simulations and the curvature model allows for a better understanding of oligomeric structures on surfaces.
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    Towards efficient initiators for two-photon induced polymerization: Fine tuning of the donor/acceptor properties
    (Cambridge : Royal Society of Chemistry, 2019) Holzer, Brigitte; Lunzer, Markus; Rosspeintner, Arnulf; Licari, Giuseppe; Tromayer, Maximilian; Naumov, Sergej; Lumpi, Daniel; Horkel, Ernst; Hametner, Christian; Ovsianikov, Aleksandr; Liska, Robert; Vauthey, Eric; Fröhlich, Johannes
    In this work we present the design, synthesis and systematic investigation of the optical properties of symmetric triphenylamine (TPA)-substituted thiophenes. The use of electron-donating (-OMe, -tBu, -Me, -TMS), -neutral (-H) or -withdrawing (-F, -CN, -SO2Me) substituents gives rise to D-A-D based two-photon absorption (2PA) chromophores. The photophysical properties of these compounds, including one-photon absorption and 2PA using two-photon-excited fluorescence, were investigated in different organic solvents with varying polarity. The maximum 2PA cross sections prove to be strongly dependent on the nature of the TPA substituent and range between ~173 GM (Goeppert-Mayer units) and 379 GM. Although most of the investigated substances also exhibit high fluorescence quantum yields, two-photon absorption screening tests of an acrylate monomer formulation revealed the efficiency of these materials as 2PA photoinitiators. These results are supported by quantum chemical calculations of the spin density distribution indicating that the mechanism of polymerization initiation using acrylate monomer is favored by strong localization of the unpaired electrons in the triplet state on the C2 carbon of the thiophene moiety. © 2019 The Royal Society of Chemistry.
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    Laminin Adsorption and Adhesion of Neurons and Glial Cells on Carbon Implanted Titania Nanotube Scaffolds for Neural Implant Applications
    (Basel : MDPI, 2022) Frenzel, Jan; Kupferer, Astrid; Zink, Mareike; Mayr, Stefan G.
    Interfacing neurons persistently to conductive matter constitutes one of the key challenges when designing brain-machine interfaces such as neuroelectrodes or retinal implants. Novel materials approaches that prevent occurrence of loss of long-term adhesion, rejection reactions, and glial scarring are highly desirable. Ion doped titania nanotube scaffolds are a promising material to fulfill all these requirements while revealing sufficient electrical conductivity, and are scrutinized in the present study regarding their neuron–material interface. Adsorption of laminin, an essential extracellular matrix protein of the brain, is comprehensively analyzed. The implantation-dependent decline in laminin adsorption is revealed by employing surface characteristics such as nanotube diameter, (Formula presented.) -potential, and surface free energy. Moreover, the viability of U87-MG glial cells and SH-SY5Y neurons after one and four days are investigated, as well as the material’s cytotoxicity. The higher conductivity related to carbon implantation does not affect the viability of neurons, although it impedes glial cell proliferation. This gives rise to novel titania nanotube based implant materials with long-term stability, and could reduce undesirable glial scarring.
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    Employing Nanostructured Scaffolds to Investigate the Mechanical Properties of Adult Mammalian Retinae Under Tension
    (Basel : Molecular Diversity Preservation International, 2020) Juncheed, Kantida; Kohlstrunk, Bernd; Friebe, Sabrina; Dallacasagrande, Valentina; Maurer, Patric; Reichenbach, Andreas; Mayr, Stefan G.; Zink, Mareike
    Numerous eye diseases are linked to biomechanical dysfunction of the retina. However, the underlying forces are almost impossible to quantify experimentally. Here, we show how biomechanical properties of adult neuronal tissues such as porcine retinae can be investigated under tension in a home-built tissue stretcher composed of nanostructured TiO2 scaffolds coupled to a self-designed force sensor. The employed TiO2 nanotube scaffolds allow for organotypic long-term preservation of adult tissues ex vivo and support strong tissue adhesion without the application of glues, a prerequisite for tissue investigations under tension. In combination with finite element calculations we found that the deformation behavior is highly dependent on the displacement rate which results in Young’s moduli of (760–1270) Pa. Image analysis revealed that the elastic regime is characterized by a reversible shear deformation of retinal layers. For larger deformations, tissue destruction and sliding of retinal layers occurred with an equilibration between slip and stick at the interface of ruptured layers, resulting in a constant force during stretching. Since our study demonstrates how porcine eyes collected from slaughterhouses can be employed for ex vivo experiments, our study also offers new perspectives to investigate tissue biomechanics without excessive animal experiments. © 2020 by the authors. Licensee MDPI, Basel, Switzerland.
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    Microstructure Evaluation and Impurities in La Containing Silicon Oxynitrides
    (Basel : MDPI, 2021) Hakeem, Abbas Saeed; Ali, Sharafat; Höche, Thomas; Drmosh, Qasem Ahmed; Khan, Amir Azam; Jonson, Bo
    Oxynitride glasses are not yet commercialised primarily due to the impurities present in the network of these glasses. In this work, we investigated the microstructure and instinctive defects in nitrogen rich La-Si-O-N glasses. Glasses were prepared by heating a powder mixture of pure La metal, Si3N4, and SiO2 in a nitrogen atmosphere at 1650-1800 °C. The microstructure and impurities in the glasses were examined by optical microscopy, scanning electron microscopy, atomic force microscopy, and transmission electron microscopy in conjunction with electron energy-loss spectroscopy. Analyses showed that the glasses contain a small amount of spherical metal silicide particles, mostly amorphous or poorly crystalline, and having sizes typically ranging from 1 µm and less. The amount of silicide was estimated to be less than 2 vol. %. There was no systematic relation between silicide formation and glass composition or preparation temperature. The microstructure examination revealed that the opacity of these nitrogen rich glasses is due to the elemental Si arise from the decomposition reaction of silicon nitride and silicon oxide, at a high temperature above ~1600 °C and from the metallic silicide particles formed by the reduction of silicon oxide and silicon nitride at an early stage of reaction to form a silicide intermetallic with the La metal.
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    Data on single pulse fs laser induced submicron bubbles in the subsurface region of soda-lime glass
    (Amsterdam [u.a.] : Elsevier, 2020) Lai, Shengying; Ehrhardt, Martin; Lorenz, Pierre; Lu, Jian; Han, Bing; Zimmer, Klaus
    Submicron bubble formation in the subsurface range of soda-lime glass is investigated. The bubbles are induced by single femtosecond laser pulse irradiation with the wavelength of λ = 775 nm, the pulse duration of tp = 150 fs and the laser beam diameter of ∼12 μm. The data shows the changes of the morphologies of the soda-lime glass after laser irradiation with different pulse energy. Moreover, the data shows the detail of the cross-section view of the bubble during the Focused ion beam (FIB) cutting. It is found that the bubbles can be formed in a rather narrow pulse energy range with the bubbles in the size of 300 nm ∼3 μm which is much smaller than the laser beam diameter. Data presented in this article are related to the research article “Submicron bubbles/voids formation in the subsurface region of soda-lime glass by single pulse fs laser-induced spallation” [1]. © 2020