4.2 Material-Mikrobiom Wechselwirkungen
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BPA unterliegt einer kontinuierlichen behördlichen Kontrolle und ist als besonders besorgniserregender Stoff (SVHC) gelistet. Besondere Besorgnis besteht hinsichtlich seines häufigen Nachweises in Oberflächengewässern, obwohl es leicht biologisch abbaubar ist. In mehreren Studien wurden die Quellen und Wege von BPA in die Umwelt untersucht, wobei festgestellt wurde, dass seine Hauptverwendung als Monomer in PC nur marginal zu den BPA-Freisetzungen in die Umwelt über seinen Lebenszyklus beiträgt.
Um die tatsächlichen Freisetzungen von BPA aus PC unter umweltrelevanten Bedingungen besser zu verstehen, wurde eine neu entwickelte Methodik (Bundesanstalt für Materialforschung und -prüfung, BAM) angewendet, die ein neuartiges beschleunigtes Bewitterungsprotokoll für Polycarbonat-Materialien in Kombination mit einem sensitiven Analysenverfahren umfasst, welches eine Bestimmung von BPA im Ultraspurenbereich ermöglicht. Das Bewitterungsprotokoll erreicht eine 13,6-fache Beschleunigung im Vergleich zu mitteleuropäischen Wetterbedingungen und simuliert Umweltstressoren (globale Strahlung, Regen, Temperaturschwankungen) in einer Bewitterungskammer, wobei gleichzeitig die BPA-Freisetzung mit einem validierten LC-MS/MS-Verfahren unter Verwendung einer organischen Isotopenverdünnungskalibrierung bestimmt wird. In parallelen Freilandversuchen wurden die Trübung und die Vergilbung („Yellowness-Index“) der zu untersuchenden Proben als Referenzparameter untersucht.
BPA unterliegt einer kontinuierlichen behördlichen Kontrolle und ist als besonders besorgniserregender Stoff (SVHC) gelistet. Besondere Besorgnis besteht hinsichtlich seines häufigen Nachweises in Oberflächengewässern, obwohl es leicht biologisch abbaubar ist. In mehreren Studien wurden die Quellen und Wege von BPA in die Umwelt untersucht, wobei festgestellt wurde, dass seine Hauptverwendung als Monomer in PC nur marginal zu den BPA-Freisetzungen in die Umwelt über seinen Lebenszyklus beiträgt.
Um die tatsächlichen Freisetzungen von BPA aus PC unter umweltrelevanten Bedingungen besser zu verstehen, wurde eine neu entwickelte Methodik (Bundesanstalt für Materialforschung und -prüfung, BAM) angewendet, die ein neuartiges beschleunigtes Bewitterungsprotokoll für Polycarbonat-Materialien in Kombination mit einem sensitiven Analysenverfahren umfasst, welches eine Bestimmung von BPA im Ultraspurenbereich ermöglicht. Das Bewitterungsprotokoll erreicht eine 13,6-fache Beschleunigung im Vergleich zu mitteleuropäischen Wetterbedingungen und simuliert Umweltstressoren (globale Strahlung, Regen, Temperaturschwankungen) in einer Bewitterungskammer, wobei gleichzeitig die BPA-Freisetzung mit einem validierten LC-MS/MS-Verfahren unter Verwendung einer organischen Isotopenverdünnungskalibrierung bestimmt wird. In parallelen Freilandversuchen wurden die Trübung und die Vergilbung („Yellowness-Index“) der zu untersuchenden Proben als Referenzparameter untersucht.
Reusable enzyme carriers are valuable for proteomic workflows, yet many supports are expensive or lack robustness. This study describes the covalent immobilization of recombinant trypsin on micrometer-sized corundum particles and assesses their performance in protein digestion and antibody analysis. The corundum surface was cleaned with potassium hydroxide, silanized with 3-aminopropyltriethoxysilane and activated with glutaraldehyde. Recombinant trypsin was then attached, and the resulting imines were reduced with sodium cyanoborohydride. Aromatic amino acid analysis (AAAA) estimated an enzyme loading of approximately 1 µg/mg. Non-specific adsorption of human plasma proteins was suppressed by blocking residual aldehydes with a Tris-glycine-lysine buffer. Compared with free trypsin, immobilization shifted the temperature optimum from 50 to 60 °C and greatly improved stability in 1 M guanidinium hydrochloride. Activity remained above 80% across several reuse cycles, and storage at 4 °C preserved functionality for weeks. When applied to digesting the NISTmAb, immobilized trypsin provided peptide yields and sequence coverage comparable to soluble enzyme and outperformed it at elevated temperatures. MALDI-TOF MS analysis of Herceptin digests yielded fingerprint spectra that correctly identified the antibody and achieved 60% sequence coverage. The combination of low cost, robustness and analytical performance makes corundum-immobilized trypsin an attractive option for research and routine proteomic workflows.
Lead halide perovskites have emerged as a highly promising class of materials for solar cells. Nevertheless, suitable procedures to analyze the exact composition of the perovskite films are rare and are not generally applicable. Here we show a simple and fast method to determine the absolute composition of mixed metal halide perovskites through a combination of nuclear magnetic resonance and total reflection X-ray fluorescence spectroscopy. The method is validated on powder mixtures and applied to thin film samples prepared by coevaporation of formamidinium iodide (FAI), CsI, PbI2 and PbBr2, allowing correlation between film composition and solar cell performance. We show that the rates of the individual precursors do not always translate linearly into film composition and that the preparation of the hole transport layer MeO-2PACz strongly influences the incorporation of FAI. Our work highlights the importance of compositional analysis and demonstrates how the developed method provides new insights into the complex coevaporation process in perovskite solar cells.
This dataset contains raw LC–MS/MS files of trypsin-digested NISTmAb acquired on a SCIEX TripleTOF 6600 mass spectrometer in DIA (SWATH) mode for antibody quantification. In addition, it includes MALDI-TOF MS peptide mass fingerprints of trypsin-digested Herceptin as well as reference spectra that can be used for antibody identification using the open-source software ABID 2.0 (https://bam.de/ABID).
The data were generated within a study demonstrating the applicability of corundum-immobilized trypsin for antibody digestion and its suitability for peptide-based LC–MS/MS quantification and MALDI-TOF MS fingerprinting–based antibody identification.
This presentation gives an overview about the competencies and the characterization possibilities of nanoparticles at BAT, based on this the development of the OECD TG 125 at BAM. It further describes research activities at BAM concerning the characterization of nanoparticles and the way to the digital representation of these characterization possibilities. It concludes with the challenges of a digital product passport (DPP) for nanomaterial based products and the need of a digital materials passport (DMP). Finally, the activities of BAM are presented which address the former mentioned challenges from ESRP and DPP.
Diese Präsentation gibt einen Überblick über die Entwicklung der Nanopartikelforschung von ca. 2005 bis heute. Beginnend mit den Besonderheiten von Nanopartikeln und der Aufnahme in den menschlichen Körper über Messmethoden bis hin zur Entwicklung einer Prüfrichtlinie im Rahmen der OECD und einem Ausblick über die absehbaren digitalen Entwicklungen.
The digital product passport
(2025)
Reusable enzyme carriers are valuable for proteomic workflows, yet many supports are expensive or lack robustness. This study describes the covalent immobilization of recombinant trypsin on micrometer-sized corundum particles and assesses their performance in protein digestion and antibody analysis. The corundum surface was cleaned with potassium hydroxide, silanized with 3-aminopropyltriethoxysilane and activated with glutaraldehyde. Recombinant trypsin was then attached, and the resulting imines were reduced with sodium cyanoborohydride. Aromatic amino acid analysis (AAAA) estimated an enzyme loading of approximately 1 µg/mg. Non-specific adsorption of human plasma proteins was suppressed by blocking residual aldehydes with a Tris-glycine-lysine buffer. Compared with free trypsin, immobilization shifted the temperature optimum from 50 to 60 °C and greatly improved stability in 1 M guanidinium hydrochloride. Activity remained above 80 % across several reuse cycles, and storage at 4 °C preserved functionality for weeks. When applied to digesting the NISTmAb, immobilized trypsin provided peptide yields and sequence coverage comparable to soluble enzyme and outperformed it at elevated temperatures. MALDI-TOF MS analysis of Herceptin digests yielded fingerprint spectra that correctly identified the antibody and achieved >60 % sequence coverage. The combination of low cost, robustness and analytical performance makes corundum-immobilized trypsin an attractive option for research and routine proteomic workflows.
Bisphenol A (BPA) is under continuous regulatory scrutiny and listed as substance of very high concern (SVHC). Particular concern is related to its frequent detection in surface waters, despite being readily biodegradable. Several studies have been conducted to investigate sources and pathways of BPA in the environment, concluding that its main use as monomer in polycarbonate (PC) contributes only marginally to environmental BPA releases over its life cycle.
To better understand the actual releases of BPA from PC under environmental conditions, a newly developed methodology (Federal Institute for Materials Research and Testing, BAM) was applied, which comprises a novel accelerated weathering protocol for polycarbonate (PC) materials, combined with an advanced analytical setup allowing for improved detection of BPA at trace level concentrations. The weathering protocol achieves a 13.6-fold acceleration compared to Central European outdoor conditions and simulates environmental stressors (global radiation, rain, temperature variations) in a laboratory weathering chamber, with simultaneous BPA release measurements using an organic isotope dilution calibration LC-MS/MS approach. Validation was performed in parallel outdoor exposure tests, by using haze and yellowness index measurements as reference parameters.
PC sample types representative of major polycarbonate applications were examined: Samples with different levels of UV-protection as used in transparent sheets used outdoor in construction or housings in Electro- and Electronic applications as well as samples with a protective coating as used in automotive applications (headlamps, glazing and construction).
Results demonstrated consistently low total BPA releases of around 0.3 mg m⁻² for samples with exposed PC surfaces, while releases from coated samples were significantly reduced by around two orders of magnitude. In all cases examined, the BPA release ceased to zero after a period of four to six weeks, equivalent to approximately 1 to 1.5 years of outdoor exposure. This suggests that potential BPA releases diminish to virtually zero after that timespan. While the newly developed test method is not suitable for routine laboratory implementation, it provides crucial quantitative data on BPA release from PC materials during accelerated environmental weathering.