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- ItemSubcritical fluid chromatography at sub-ambient temperatures for the chiral resolution of ketamine metabolites with rapid-onset antidepressant effects(Basel : MDPI, 2019) Hofstetter, Robert K.; Potlitz, Felix; Schulig, Lukas; Kim, Simon; Hasan, Mahmoud; Link, AndreasChiral metabolites of ketamine exerting rapid-onset yet sustained antidepressant effects may be marketed directly in the future, but require chemo- and enantio-selective chromatographic methods for quality assurance and control. The chromatographic behavior of S-/R-ketamine, S-/R-norketamine, S-/R-dehydronorketamine, and (2R,6R)-/(2S,6S)-hydroxynorketamine in supercritical fluid chromatography (SFC) was investigated computationally and experimentally with the aim of identifying problematic pairs of enantiomers and parameters for chiral resolution. Retention on three different polysaccharide-based chiral stationary phases (Lux Amylose-2, i-Amylose-3, and i-Cellulose-5) provided new information on the significance of halogen atoms as halogen bond donors and hydrogen bond acceptors for enantioselectivity, which could be corroborated in silico by molecular docking studies. Modifiers inversely affected enantioselectivity and retention. Methanol yielded lower run times but superior chiral resolution compared to 2-propanol. Lower temperatures than those conventionally screened did not impair phase homogeneity but improved enantioresolution, at no cost to reproducibility. Thus, sub-ambient temperature subcritical fluid chromatography (SubFC), essentially low-temperature HPLC with subcritical CO2, was applied. The optimization of the SubFC method facilitated the chiral separation of ketamine and its metabolites, which was applied in combination with direct injection and online supercritical fluid extraction to determine the purity of pharmaceutical ketamine formulations for proof of concept. © 2019 by the authors.
- ItemSynthesis of hydroxy-sodalite/cancrinite zeolites from calcite-bearing kaolin for the removal of heavy metal ions in aqueous media(Basel : MDPI, 2019) Esaifan, Muayad; Warr, Laurence N.; Gratho, Georg; Meyer, Tammo; Schafmeister, Maria-Theresia; Kruth, Angela; Testrich, HolgerA hydroxy-sodalite/cancrinite zeolite composite was synthesized from low-grade calcite-bearing kaolin by hydrothermal alkali-activation method at 160 °C for 6 h. The effect of calcite addition on the formation of the hydroxy-sodalite/cancrinite composite was investigated using artificial mixtures. The chemical composition and crystal morphology of the synthesized zeolite composite were characterized by X-ray powder diffraction, infrared spectroscopy, scanning electron microscopy, and N2 adsorption/desorption analyses. The average specific surface area is around 17–20 m2·g−1, whereas the average pore size lies in the mesoporous range (19–21 nm). The synthesized zeolite composite was used as an adsorbent for the removal of heavy metals in aqueous solutions. Batch experiments were employed to study the influence of adsorbent dosage on heavy metal removal efficiency. Results demonstrate the effective removal of significant quantities of Cu, Pb, Ni, and Zn from aqueous media. A comparative study of synthesized hydroxy-sodalite and hydroxy-sodalite/cancrinite composites revealed the latter was 16–24% more efficient at removing heavy metals from water. The order of metal uptake efficiency for these zeolites was determined to be Pb > Cu > Zn > Ni. These results indicate that zeolite composites synthesized from natural calcite-bearing kaolin materials could represent effective and low-cost adsorbents for heavy metal removal using water treatment devices in regions of water shortage.
- ItemMineral-Based Coating of Plasma-Treated Carbon Fibre Rovings for Carbon Concrete Composites with Enhanced Mechanical Performance(Basel : MDPI, 2017-3-29) Schneider, Kai; Lieboldt, Matthias; Liebscher, Marco; Fröhlich, Maik; Hempel, Simone; Butler, Marko; Schröfl, Christof; Mechtcherine, ViktorSurfaces of carbon fibre roving were modified by means of a low temperature plasma treatment to improve their bonding with mineral fines; the latter serving as an inorganic fibre coating for the improved mechanical performance of carbon reinforcement in concrete matrices. Variation of the plasma conditions, such as gas composition and treatment time, was accomplished to establish polar groups on the carbon fibres prior to contact with the suspension of mineral particles in water. Subsequently, the rovings were implemented in a fine concrete matrix and their pull-out performance was assessed. Every plasma treatment resulted in increased pull-out forces in comparison to the reference samples without plasma treatment, indicating a better bonding between the mineral coating material and the carbon fibres. Significant differences were found, depending on gas composition and treatment time. Microscopic investigations showed that the samples with the highest pull-out force exhibited carbon fibre surfaces with the largest areas of hydration products grown on them. Additionally, the coating material ingresses into the multifilament roving in these specimens, leading to better force transfer between individual carbon filaments and between the entire roving and surrounding matrix, thus explaining the superior mechanical performance of the specimens containing appropriately plasma-treated carbon roving.
- ItemDeposition of Antimicrobial Copper-Rich Coatings on Polymers by Atmospheric Pressure Jet Plasmas(Basel : MDPI, 2016) Kredl, Jana; Kolb, Juergen F.; Schnabel, Uta; Polak, Martin; Weltmann, Klaus-Dieter; Fricke, KatjaInanimate surfaces serve as a permanent reservoir for infectious microorganisms, which is a growing problem in areas in everyday life. Coating of surfaces with inorganic antimicrobials, such as copper, can contribute to reduce the adherence and growth of microorganisms. The use of a DC operated air plasma jet for the deposition of copper thin films on acrylonitrile butadiene styrene (ABS) substrates is reported. ABS is a widespread material used in consumer applications, including hospitals. The influence of gas flow rate and input current on thin film characteristics and its bactericidal effect have been studied. Results from X-ray photoelectron spectroscopy (XPS) and atomic force microscopy confirmed the presence of thin copper layers on plasma-exposed ABS and the formation of copper particles with a size in the range from 20 to 100 nm, respectively. The bactericidal properties of the copper-coated surfaces were tested against Staphylococcus aureus. A reduction in growth by 93% compared with the attachment of bacteria on untreated samples was observed for coverage of the surface with 7 at. % copper.
- ItemRES-Q-Trace: A Mobile CEAS-Based Demonstrator for Multi-Component Trace Gas Detection in the MIR(Basel : MDPI, 2018-6-27) Lang, Norbert; Macherius, Uwe; Zimmermann, Henrik; Glitsch, Sven; Wiese, Mathias; Röpcke, Jürgen; van Helden, Jean-Pierre H.Sensitive trace gas detection plays an important role in current challenges occurring in areas such as industrial process control and environmental monitoring. In particular, for medical breath analysis and for the detection of illegal substances, e.g., drugs and explosives, a selective and sensitive detection of trace gases in real-time is required. We report on a compact and transportable multi-component system (RES-Q-Trace) for molecular trace gas detection based on cavity-enhanced techniques in the mid-infrared (MIR). The RES-Q-Trace system can operate four independent continuous wave quantum or interband cascade lasers each combined with an optical cavity. Twice the method of off-axis cavity-enhanced absorption spectroscopy (OA-CEAS) was used, twice the method of optical feedback cavity-enhanced absorption spectroscopy (OF-CEAS), respectively. Multi-functional software has been implemented (i) for the general system control; (ii) to drive the four different laser sources and (iii) to analyze the detector signals for concentration determination of several molecular species. For the validation of the versatility and the performance of the RES-Q-Trace instrument the species NO, N2O, CH4, C2H4 and C3H6O, with relevance in the fields of breath gas analysis and the detection of explosives have been monitored in the MIR with detection limits at atmospheric pressure in the ppb and ppt range.
- ItemPlasma polymerized allylamine-the unique cell-attractive nanolayer for dental implant materials(Basel : MDPI, 2019) Nebe, J. Barbara; Rebl, Henrike; Schlosser, Michael; Staehlke, Susanne; Gruening, Martina; Weltmann, Klaus-Dieter; Walschus, Uwe; Finke, BirgitBiomaterials should be bioactive in stimulating the surrounding tissue to accelerate the ingrowth of permanent implants. Chemical and topographical features of the biomaterial surface affect cell physiology at the interface. A frequently asked question is whether the chemistry or the topography dominates the cell-material interaction. Recently, we demonstrated that a plasma-chemical modification using allylamine as a precursor was able to boost not only cell attachment and cell migration, but also intracellular signaling in vital cells. This microwave plasma process generated a homogenous nanolayer with randomly distributed, positively charged amino groups. In contrast, the surface of the human osteoblast is negatively charged at −15 mV due to its hyaluronan coat. As a consequence, we assumed that positive charges at the material surface—provoking electrostatic interaction forces—are attractive for the first cell encounter. This plasma-chemical nanocoating can be used for several biomaterials in orthopedic and dental implantology like titanium, titanium alloys, calcium phosphate scaffolds, and polylactide fiber meshes produced by electrospinning. In this regard, we wanted to ascertain whether plasma polymerized allylamine (PPAAm) is also suitable for increasing the attractiveness of a ceramic surface for dental implants using Yttria-stabilized tetragonal zirconia.
- ItemMorphology, Optical Properties and Photocatalytic Activity of Photo- and Plasma-Deposited Au and Au/Ag Core/Shell Nanoparticles on Titania Layers(Basel : MDPI, 2018-7-6) Müller, Alexander; Peglow, Sandra; Karnahl, Michael; Kruth, Angela; Junge, Henrik; Brüser, Volker; Scheu, ChristinaTitania is a promising material for numerous photocatalytic reactions such as water splitting and the degradation of organic compounds (e.g., methanol, phenol). Its catalytic performance can be significantly increased by the addition of co-catalysts. In this study, Au and Au/Ag nanoparticles were deposited onto mesoporous titania thin films using photo-deposition (Au) and magnetron-sputtering (Au and Au/Ag). All samples underwent comprehensive structural characterization by grazing incidence X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Nanoparticle distributions and nanoparticle size distributions were correlated to the deposition methods. Light absorption measurements showed features related to diffuse scattering, the band gap of titania and the local surface plasmon resonance of the noble metal nanoparticles. Further, the photocatalytic activities were measured using methanol as a hole scavenger. All nanoparticle-decorated thin films showed significant performance increases in hydrogen evolution under UV illumination compared to pure titania, with an evolution rate of up to 372 μL H2 h−1 cm−2 representing a promising approximately 12-fold increase compared to pure titania.
- ItemPlasma-treated air and water-assessment of synergistic antimicrobial effects for sanitation of food processing surfaces and environment(Basel : MDPI, 2019) Schnabel, Uta; Handorf, Oliver; Yarova, Kateryna; Zessin, Björn; Zechlin, Susann; Sydow, Diana; Zellmer, Elke; Stachowiak, Jörg; Andrasch, Mathias; Below, Harald; Ehlbeck, JörgThe synergistic antimicrobial effects of plasma-processed air (PPA) and plasma-treated water (PTW), which are indirectly generated by a microwave-induced non-atmospheric pressure plasma, were investigated with the aid of proliferation assays. For this purpose, microorganisms (Listeria monocytogenes, Escherichia coli, Pectobacterium carotovorum, sporulated Bacillus atrophaeus) were cultivated as monocultures on specimens with polymeric surface structures. Both the distinct and synergistic antimicrobial potential of PPA and PTW were governed by the plasma-on time (5–50 s) and the treatment time of the specimens with PPA/PTW (1–5 min). In single PTW treatment of the bacteria, an elevation of the reduction factor with increasing treatment time could be observed (e.g., reduction factor of 2.4 to 3.0 for P. carotovorum). In comparison, the combination of PTW and subsequent PPA treatment leads to synergistic effects that are clearly not induced by longer treatment times. These findings have been valid for all bacteria (L. monocytogenes > P. carotovorum = E. coli). Controversially, the effect is reversed for endospores of B. atrophaeus. With pure PPA treatment, a strong inactivation at 50 s plasma-on time is detectable, whereas single PTW treatment shows no effect even with increasing treatment parameters. The use of synergistic effects of PTW for cleaning and PPA for drying shows a clear alternative for currently used sanitation methods in production plants. Highlights: Non-thermal atmospheric pressure microwave plasma source used indirect in two different modes—gaseous and liquid; Measurement of short and long-living nitrite and nitrate in corrosive gas PPA (plasma-processed air) and complex liquid PTW (plasma-treated water); Application of PTW and PPA in single and combined use for biological decontamination of different microorganisms.
- ItemApplying Quantum Cascade Laser Spectroscopy in Plasma Diagnostics(Basel : MDPI, 2016) Röpcke, Jürgen; Davies, Paul; Hamann, Stephan; Hannemann, Mario; Lang, Norbert; van Helden, Jean-PierreThe considerably higher power and wider frequency coverage available from quantum cascade lasers (QCLs) in comparison to lead salt diode lasers has led to substantial advances when QCLs are used in pure and applied infrared spectroscopy. Furthermore, they can be used in both pulsed and continuous wave (cw) operation, opening up new possibilities in quantitative time resolved applications in plasmas both in the laboratory and in industry as shown in this article. However, in order to determine absolute concentrations accurately using pulsed QCLs, careful attention has to be paid to features like power saturation phenomena. Hence, we begin with a discussion of the non-linear effects which must be considered when using short or long pulse mode operation. More recently, cw QCLs have been introduced which have the advantage of higher power, better spectral resolution and lower fluctuations in light intensity compared to pulsed devices. They have proved particularly useful in sensing applications in plasmas when very low concentrations have to be monitored. Finally, the use of cw external cavity QCLs (EC-QCLs) for multi species detection is described, using a diagnostics study of a methane/nitrogen plasma as an example. The wide frequency coverage of this type of QCL laser, which is significantly broader than from a distributed feedback QCL (DFB-QCL), is a substantial advantage for multi species detection. Therefore, cw EC-QCLs are state of the art devices and have enormous potential for future plasma diagnostic studies.
- ItemPlasma-derived reactive species shape a differentiation profile in human monocytes(Basel : MDPI, 2019) Freund, Eric; Moritz, Juliane; Stope, Matthias; Seebauer, Christian; Schmidt, Anke; Bekeschus, SanderBackground: Monocyte-derived macrophages are key regulators and producers of reactive oxygen and nitrogen species (ROS/RNS). Pre-clinical and clinical studies suggest that cold physical plasma may be beneficial in the treatment of inflammatory conditions via the release of ROS/RNS. However, it is unknown how plasma treatment affects monocytes and their differentiation profile. Methods: Naïve or phorbol-12-myristate-13-acetate (PMA)-pulsed THP-1 monocytes were exposed to cold physical plasma. The cells were analyzed regarding their metabolic activity as well as flow cytometry (analysis of viability, oxidation, surface marker expression and cytokine secretion) and high content imaging (quantitative analysis of morphology. Results: The plasma treatment affected THP-1 metabolisms, viability, and morphology. Furthermore, a significant modulation CD55, CD69, CD271 surface-expression and increase of inflammatory IL1β, IL6, IL8, and MCP1 secretion was observed upon plasma treatment. Distinct phenotypical changes in THP-1 cells arguing for a differentiation profile were validated in primary monocytes from donor blood. As a functional outcome, plasma-treated monocytes decreased the viability of co-cultured melanoma cells to a greater extent than their non-treated counterparts. Conclusions: Our results suggest plasma-derived ROS/RNS shaped a differentiation profile in human monocytes as evidenced by their increased inflammatory profile (surface marker and cytokines) as well as functional outcome (tumor toxicity). © 2019 by the authors.