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Organisationseinheit der BAM
Untersuchungen zur Charakterisierung des Abbaus von Polylactiden mittels 2D-HPLC und MALDI-TOF-MS
(1995)
Various dibutyltin derivatives were polycondensed with aliphatic ,-dicarboxylic acids having chain lengths from 4 (succinic acid) to 22 carbon atoms. White crystalline products were obtained from all experiments, and the structure of the products was independent of the synthetic method. Viscosity measurements revealed low molecular weights (n 1 500 Da) in all cases. Vapor pressure osmometry (VPO) measurements and matrix-assisted laser desorption time-of-flight (MALDI-TOF) mass spectrometry proved that cyclic dimers and trimer were formed from dicarboxylic acids having 6 to 16 carbons, but mainly the monomeric cycle from docosane dioic acid. Heating to 250°C did not change the structure. Therefore, the results indicate that the macrocycles are the result of a thermodynamically controlled ring-closing polycondensation. This means that linear high-molecular weight poly(dibutyltin dicarboxylate)s cannot exist above room temperature.
Poly(ether sulfone)s were prepared by polycondensation of silylated 4-tert-butylcatechol and 4,4?-difluorodiphenylsulfone in N-methylpyrrolidone. The feed ratio and the reaction time were varied to study the influence of stoichiometry and conversion on molecular weight and extent of cyclization. Molecular weights and molecular weight distributions (MWD)s were characterized by SEC measurements calibrated with polystyrene. Light scattering confirmed that calibration with polystyrene gives reasonable results and revealed a tendency towards a bimodal MWD for the samples rich in cycles. The MALDI-TOF mass spectrometry indicated that the extent of cyclization increased with higher conversion and with optimization of the stoichiometry. This interpretation was confirmed by 1H NMR endgroup analyses. For the samples with the highest molar masses only mass peaks of cycles were found, which were detectable up to 20 000 Da before and up to 27 000 Da after fractionation. Via the pseudo-high dilution method low molar mass poly(ether sulfone) containing more than 95 mol% of cycles were prepared, and even these low molar mass samples had broad MWDs. DSC measurements indicated that the glass transition temperatures depend on the structure of the endgroups and increase with higher fractions of cycles.
3,5-Bis(4-fluorobenzoyl)phenol was polycondensed under various reaction conditions. Low molecular weights were obtained (Mn < 8000 Da), and MALDI-TOF mass spectrometry indicated that the chain growth was limited by cyclization. In the best mass spectra the cyclic, hyperbranched poly(ether ketone)s were detectable up to masses around 14 000 Da. When 4,4'-difluordiphenyl sulfone was added, star-shaped polymers having a diphenyl sulfone star center were formed, but cyclization was not completely suppressed. The results were compared to those obtained from "linear polycondensations" based on 4,4'-difluorobenzophenone (DFBP) and 4-tert-butylcatechol or bisphenol A. The poly(ether ketone)s of DFBP had also low molecular weights and contained high fractions of cycles. It is concluded that also in the case of hyperbranched polymers cyclization competes with propagation at any stage of the polycondensation at any concentration. Therefore, the fundamental trend of any "abn" polycondensation is the formation of star-shaped polymers having a cyclic core and hyperbranched star arms.
Purpose: To determine the distensibility and elastic characteristics of the optic nerve sheath for development of a basic understanding of ultrasound studies aimed to measure optic nerve sheath diameter (ONSD) for detection of acutely elevated intracranial pressure (ICP).
Methods: Isolated human optic nerves preparations obtained from autopsies were submitted to predefined pressure alterations, and consecutive changes in ONSD were measured by B-scan ultrasound under defined conditions.
Results: Following submission to pressure, the diameter of the nerve sheath increased up to 140% of its baseline value. The increase (mean 1.97 mm, SD 0.52 mm) corresponded to the magnitude of pressure steps measured in the perineural subarachnoidal space (SAS). Similarly, the ONSD declined in each of the preparations within a few minutes after the optic nerve was decompressed. However, it did not reach its baseline value again when pressure loads of 45–55 mmHg or more had been applied.
Conclusions: The elasticity of the anterior sheath of the optic nerve is sufficient for the detection of pressure changes in the SAS especially for upward pressure steps. This is basically important for the application of clinical monitoring of the sheath diameter to facilitate the identification of patients with elevated ICP non-invasively (screening). However, further implementation of this procedure in neurointensive care and emergency medicine has to consider that the sheath diameter reversibility may be impaired after episodes of prolonged intracranial hypertension and a model for hysteresis is proposed.
Wer mit Laserstrahlung zu tun hat, sollte vor allem auf den Schutz seiner Augen achten, denn die Netzhaut ist eines der empfindlichsten Gewebe des menschlichen Körpers. Auch die Hornhaut des Auges kann durch Laserstrahlung gefährdet sein. Sie hat eine Dicke von nur etwa 0,5 mm. Der Schutz der Augen vor Laserstrahlung ist durch verschiedene Maßnahmen möglich.
The European laser safety standards EN 207, EN 208, and EN 12254 each contain an annex B, which serves as a guidance for the selection of products. These annexes are informative only and are therefore not binding. As there are a variety of hazard scenarios, it is not recommended to change these annexes to a normative status, through which they would become mandatory. Instead, it is recommended to allow users to apply their own skills and know-how in selecting appropriate products, justifying where and why they deviate from the guidance in the standards. This paper explains the background on which the guidance for selection in the annexes of the standards is based and shows physically meaningful leeway.
The thermal degradation behavior of poly(vinyl chloride) (PVC) and poly(N-vinylpyrrolidone) (PVP) blends was investigated using potentiometric measurements of the released HCl gas during the degradation process, estimating the degree of discoloration of the degraded samples and measuring the thermal stability values (Ts) values. The influence of the PVP percentage in the blend and, moreover, the addition of commercial dibasic lead carbonate stabilizer to the blend on its thermal stability was studied. It was found that the dehydrochlorination rate of the blend was promoted by increasing the PVP concentration in the blend.
MALDI-TOF-MS-based identification of monoclonal murine anti-SARS-CoV-2 antibodies within one hour
(2022)
During the SARS-CoV-2 pandemic, many virus-binding monoclonal antibodies have been developed for clinical and diagnostic purposes. This underlines the importance of antibodies as universal bioanalytical reagents. However, little attention is given to the reproducibility crisis that scientific studies are still facing to date. In a recent study, not even half of all research antibodies mentioned in publications could be identified at all. This should spark more efforts in the search for practical solutions for the traceability of antibodies. For this purpose, we used thirty-five monoclonal antibodies against SARS-CoV-2 to demonstrate how sequence-independent antibody identification can be achieved by simple means applied onto the protein. First, we examined the intact and light chain masses of the antibodies relative to the reference material NIST-mAb 8671. Already half of the antibodies could be identified based solely on these two parameters. In addition, we developed two complementary peptide mass fingerprinting methods with MALDI-TOF-MS that can be performed in 45 minutes and had a combined sequence coverage of over 80%. One method is based on the partial acidic hydrolysis of the protein by 5 mM of sulfuric acid at 99 °C. Furthermore, we established a fast way for a tryptic digest without an alkylation step. We were able to show that the distinction of clones is possible simply by a brief visual comparison of the mass spectra. In this work, two clones originating from the same immunization gave the same fingerprints. Later, a hybridoma sequencing confirmed the sequence identity of these sister clones. In order to automate the spectral comparison for larger libraries of antibodies, we developed the online software ABID 2.0 (https://gets.shinyapps.io/ABID/). This open-source software determines the number of matching peptides in the fingerprint spectra. We propose that publications and other documents critically relying on monoclonal antibodies with unknown amino acid sequences should include at least one antibody fingerprint. By fingerprinting an antibody in question, its identity can be confirmed by comparison with a library spectrum at any time and context.
Indium islands on molybdenum coated glass can be grown in ordered arrays by surface structuring using a femtosecond laser. The effect of varying the molybdenum coated glass substrate temperature and the indium deposition rate on island areal density, volume and geometry is investigated and evaluated in a physical vapor deposition (PVD) process. The joined impact of growth conditions and spacing of the femtosecond laser structured spots on the arrangement and morphology of indium islands is demonstrated. The results yield a deeper understanding of the island growth and its precise adjustment to industrial requirements, which is indispensable for a technological application of such structures at a high throughput, for instance as precursors for the preparation of Cu(In,Ga)Se2 micro concentrator solar cells.
The ultrafast laser ablation of silicon has been investigated experimentally and theoretically. The theoretical description is based on molecular dynamics (MD) simulations combined with a microscopic electronic model. We determine the thresholds of melting and ablation for two different pulse durations =20 and 500 fs. Experiments have been performed using 100 Ti:Sap-phire laser pulses per spot in air environment. The ablation thresholds were determined for pulses with a duration of 25 and 400 fs, respectively. Good agreement is obtained between theory and experiment.