TY - JOUR A1 - Wimmer, L A1 - Hoang, M V N A1 - Schwarzinger, J A1 - Jovanovic, V A1 - Adelkovic, B A1 - Velickovic, T C A1 - Meisel, T C A1 - Waniek, T A1 - Weimann, Christiane A1 - Altmann, Korinna A1 - Dailey, L A T1 - A quality-by-design inspired approach to develop PET and PP nanoplastic test materials for use in in vitro and in vivo biological assays N2 - Micro- and nanoplastics have become environmental pollutants of concern, receiving increased attention from consumers, scientists, and policymakers. The lack of knowledge about possible impacts on wildlife and human health requires further research, for which well-characterized testmaterials are needed. A quality-bydesign (QbD) driven approachwas used to produce sterile, endotoxinmonitored nanoplastics of polyethylene terephthalate (PET) and polypropylene (PP) with a size fraction of >90% below 1 μm and high yield of >90%. Glycerol was used as a versatile and biocompatible liquid storage medium which requires no further exogenous dispersing agent andmaintained colloidal stability, sterility (0 CFU mL−1), and low endotoxin levels (<0.1 EU mL−1) for more than one year of storage at room temperature. Further, the glycerol vehicle showed no biological effect on the tested human bronchial cell line Calu-3 up to 0.8% (w/v). Given the concentration of 40 mg g−1 nanoplastics in the glycerol stock, this corresponds to a nanoplastic concentration of 320 μg mL−1. The surfactant-free nanoplastics are dispersible in bio-relevant media from the glycerol stock without changing size characteristics and are suitable for in vitro and in vivo research. KW - Microplastics KW - Reference materials KW - Nanoplastics KW - Polymer 3R KW - Glycerol PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629934 DO - https://doi.org/10.1039/D4EN01186D SN - 2051-8161 VL - 12 IS - 5 SP - 2667 EP - 2686 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-62993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Starkholm, A. A1 - Al-Sabbagh, Dominik A1 - Sarisozen, S A1 - von Reppert, A A1 - Rössle, M A1 - Ostermann, Markus A1 - Unger, E A1 - Emmerling, Franziska A1 - Kloo, L A1 - Svensson, P A1 - Lang, F A1 - Maslyanchuk, O. T1 - Green Fabrication of Sulfonium-Containing Bismuth Materials for High-Sensitivity X-Ray Detection N2 - Organic–inorganic hybrid materials based on lead and bismuth have recently been proposed as novel X- and gamma-ray detectors for medical imaging, non-destructive testing, and security, due to their high atomic numbers and facile preparation compared to traditional materials like amorphous selenium and Cd(Zn)Te. However, challenges related to device operation, excessively high dark currents, and long-term stability have delayed commercialization. Here, two novel semiconductors incorporating stable sulfonium cations are presented, [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5, synthesized via solvent-free ball milling and fabricated into dense polycrystalline pellets using cold isostatic compression, two techniques that can easily be upscaled, for X-ray detection application. The fabricated detectors exhibit exceptional sensitivities (14 100–15 190 µC Gyair−1 cm−2) and low detection limits (90 nGyair s−1 for [(CH3CH2)3S]6Bi8I30 and 78 nGyair s−1 for [(CH3CH2)3S]AgBiI5), far surpassing current commercial detectors. Notably, they maintain performance after 9 months of ambient storage. The findings highlight [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5 as scalable, cost-effective and highly stable alternatives to traditional semiconductor materials, offering great potential as X-ray detectors in medical and security applications. KW - Mechanochemistry KW - X-ray detectors PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630306 DO - https://doi.org/10.1002/adma.202418626 SP - 1 EP - 10 PB - Wiley VHC-Verlag AN - OPUS4-63030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodríguez-Sánchez, Noelia A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska A1 - Prinz, Carsten A1 - Prieto-Laria, P. A1 - Ruiz-Salvador, A.R. A1 - Ballesteros, M. T1 - Engineering a multivariate cobalt metal–organic framework for high photocatalytic activity: the impact of mixed ligands and metal incorporation in a visible light-driven heterogeneous photo-Fenton reaction for water treatment N2 - Metal–organic frameworks (MOFs) have attracted increasing attention for the removal of organic pollutants in wastewater via photocatalysis. Here, we design a multivariate modification of ZIF-9 to tune its electronic properties for use in visible light photocatalysis. A controllable synthesis of ZIF-9 and its multivariate forms with the incorporation of copper and the 2-imidazolecarboxaldehyde (ica) ligand was carried out. The materials are tested for the removal of the model dye methylene blue (MB) by a heterogeneous photo-Fenton-like reaction at neutral pH and room temperature. Cu-ZIF-9-ica (UPO-3) shows high photocatalytic activity under both visible and ultraviolet A (UVA) light, achieving 94% MB degradation in 45 min, compared to 65% MB degradation in 120 min using bare ZIF-9. The study revealed a first-order rate constant of 0.0475 min−1 for Cu-ZIF-9-ica compared to 0.0088 min−1 for ZIF-9 under visible light. The improvement of the catalyst was clearly attributed to the co-incorporation of Cu and the ica ligand in the MOF, which reduces the band gap, in agreement with DFT calculations. Reproducibility and recyclability tests proved that Cu-ZIF-9-ica can be used for at least 3 cycles without a significant loss of efficiency, making it a promising material for the study and application of wastewater treatment. KW - Metal-Organic Framework (MOF) KW - Heterogeneous photo-Fenton KW - ZIF-9 KW - Methylene Blue PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630797 DO - https://doi.org/10.1039/d4na00954a SN - 2516-0230 VL - 7 IS - 8 SP - 2255 EP - 2265 PB - Royal Society of Chemistry AN - OPUS4-63079 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Visileanu, Emilia A1 - Catalin Grosu, Marian A1 - Tiberiu Miclea, Paul A1 - Altmann, Korinna A1 - Brossell, Dirk T1 - Methods for the collection and characterization of airborne particles in the textile industry N2 - Airborne particulate matter is one of the main air pollutants. Their impact on mortality, and the occurrence of pulmonary and cardiovascular complications, have been the subject of numerous studies. Airborne particles are complex mixtures of organic and inorganic substances from different sources of particle emissions. Particulate Matter (PM) particles are classified according to their aerodynamic diameter expressed in µm and can vary from coarse (PM 10) to fine (less than PM 2.5). These diameter considerations are fundamental because they condition the penetration of particles into the bronchopulmonary system and the body. In recent years, there has been an interest in so-called “ultra-fine” particles, with a diameter of 0.1 µm (or 100 nm), or PM 0.1. They are nanoparticles and their impact on human health is not yet clear.With more than 1.5 million employees, textiles and clothing is a diverse sector that plays an important role in the European manufacturing industry, producing a turnover of €162 billion.An important component of the solid particles that generate air pollution in the textile industry is microplastics (MP) and nano plastics (NP), which also include microfibers (<5mm) and nanofibers (<100 nm), respectively. The particles released into the air during fiber and yarn processing range from 1 µg/m3 to 50 µg/m3.The paper presents the results of the determination of indoor and outdoor air concentration levels in textile companies, to identify the areas with the highest concentration level, by using an online recording system such as the Laser Aerosol Spectrometer MINI LAS model 11-E. The total concentration level TSP (µg/m3), the fractions PM 10(µg/m3), PM 2.5(µg/m3), PM1(µg/m3), as well as the total number of particles TC (1/l), were shown. It was noted that TSP is approximately at the same level both indoors and outdoors, but the fractions of PM10, PM2.5, and PM1 have much higher values indoors than outdoors with possible consequences on workers' health.The next step was the collection of fibers, namely micro and nano plastic particles from the vicinity of the workplaces of polyester, polyamide, and polypropylene fibers processing units in the textile industry in Romania, to obtain a sufficient quantity for laboratory analysis to determine the size and shape of the particles as well as their chemical composition. Two types of pumps were used, differentiated by their operating parameters: TECORA SKYPOST with airflow of 38 l/min and GILAIRPLUS with airflow 2l/min. Filters made of different materials with different diameters and pore sizes were used, namely: quartz filters (ø 47 mm, and ø 37 mm) on a TECORA SKYPOST type pump, polycarbonate nucleopore coated with a gold membrane (ø 25 mm) and silica filter (ø 9 mm) on GILAIRPLUS type pump.Using descriptive statistics, the calculation of correlation coefficients highlighted a strong correlation between the variables: "Collected mass/ Air concentration" and "Collected mass/ Air volume" for all diameters of the filters.The highest collected particle volume, determined by weighing the filters before and after collection, was obtained with the quartz filters (ø 47 mm) at an airflow of 38 l/min. The particles collected (polyester, polyamide, polypropylene) in the first stage were analyzed by SEM and thermogravimetric and it was found that the quartz filters absorbed the particles inside, with very few remaining on the surface. Thus no known methods can be used to perform analysis for particles collected on quartz filters. The number of particles on the filters was insufficient for analysis either because of the collection parameters used or because of the loss of particles during transport. As a result, in the next step, the use of 9 mm Si filters using the GILAIRPLUS pump at an airflow rate of 2l/min was chosen.To improve the transport conditions and avoid the loss of the particles and keep them on the surface of the filters, two methods were applied:- after weighing the filters were reintroduced into the collection pump holder;- a filtration system for airborne micro-nano plastics was designed and manufactured to selectively collect and transport PM10 and PM1 particles collected on SI filters.In both cases, SEM, Raman mapping, and GS-MS microscopy were used for analysis.Several times more PM10 than PM1 (74.5µg compared to 12.5 µg) was found. In all cases, both particles and fibers showed the same Raman fingerprint.The GS-MS analyses showed some contamination of the workspaces with particles other than the processed fibers. The presence of non-notifiable substances was also observed.The most viable filters are Si filters with a pore size of 10 microns to 1 micron and the use of the selected collection and transport filter system. In the following a filter system will be applied for collection on Au membrane-coated polycarbonate filters. T2 - 5th International Conference on Human Systems Engineering and Design: Future Trends and Applications (IHSED 2023) KW - Microplastics KW - Textiles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624442 DO - https://doi.org/10.54941/ahfe1004132 VL - 112 SP - 212 EP - 223 PB - AHFE International AN - OPUS4-62444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Emmerling, Franziska ED - Rogge, Andreas ED - Meng, Birgit T1 - Exploring new materials for Green Intelligent Building - How can our BAMline help? N2 - In the scope of exploring and characterizing new materials related to Green Intelligent Building (GIB), we will provide an overview of the X-ray spectroscopy and diffraction analytical methods available at the BAMline /1/. and Myspot beamlines. These are two universal beamlines at the Berlin Synchrotron BESSY-II, where BAM has access and supervision role. Overarching electronic and structural properties at different time and length scales, such measurements enable a real-time characterization of materials properties. We will show-case in situ and ex situ deterioration and hydration studies on cement-based constructure materials. T2 - 11. Jahrestagung des DAfStb mit 63. Forschungskolloquium der BAM Green Intelligent Building CY - Berlin, Germany DA - 16.10.2024 KW - BAMline KW - Scope of exploring KW - Green intelligent building PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612882 SN - 978-3-9818564-7-7 SP - 30 EP - 36 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-61288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Snellings, J. A1 - Adams, L. C. A1 - Gottheil, P. A1 - Mangarova, D. B. A1 - Heyl, J. L. A1 - Kaufmann, Jan Ole A1 - Moeckel, J. A1 - Brangsch, J. A1 - Auer, T. A. A1 - Collettini, F. A1 - Sauer, F. A1 - Hamm, B. A1 - Käs, J. A1 - Sack, I. A1 - Makowski, M. R. A1 - Braun, J. T1 - Sensitivity of magnetic resonance elastography to extracellular matrix and cell motility in human prostate cancer cell line-derived xenograft models N2 - Prostate cancer (PCa) is a significant health problem in the male population of the Western world. Magnetic resonance elastography (MRE), an emerging medical imaging technique sensitive to mechanical properties of biological tissues, detects PCa based on abnormally high stiffness and viscosity values. Yet, the origin of these changes in tissue properties and how they correlate with histopathological markers and tumor aggressiveness are largely unknown, hindering the use of tumor biomechanical properties for establishing a noninvasive PCa staging system. To infer the contributions of extracellular matrix (ECM) components and cell motility, we investigated fresh tissue specimens from two PCa xenograft mouse models, PC3 and LNCaP, using magnetic resonance elastography (MRE), diffusion-weighted imaging (DWI), quantitative histology, and nuclear shape analysis. Increased tumor stiffness and impaired water diffusion were observed to be associated with collagen and elastin accumulation and decreased cell motility. Overall, LNCaP, while more representative of clinical PCa than PC3, accumulated fewer ECM components, induced less restriction of water diffusion, and exhibited increased cell motility, resulting in overall softer and less viscous properties. Taken together, our results suggest that prostate tumor stiffness increases with ECM accumulation and cell adhesion - characteristics that influence critical biological processes of cancer development. MRE paired with DWI provides a powerful set of imaging markers that can potentially predict prostate tumor development from benign masses to aggressive malignancies in patients. Statement of significance: Xenograft models of human prostate tumor cell lines, allowing correlation of microstructure-sensitive biophysical imaging parameters with quantitative histological methods, can be investigated to identify hallmarks of cancer. KW - Magnetic resonance elastography KW - Quantitative histology KW - Prostate cancer KW - Stiffness KW - Fluidity KW - Apparent diffusion coefficient KW - Collagen KW - Elastin KW - Nuclear shape PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618361 DO - https://doi.org/10.1016/j.bioadv.2024.213884 SN - 2772-9508 VL - 161 SP - 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-61836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mangarova, Dilyana Branimirova A1 - Reimann, Carolin A1 - Kaufmann, Jan Ole A1 - Möckel, Jana A1 - Kader, Avan A1 - Adams, Lisa Christine A1 - Ludwig, Antje A1 - Onthank, David A1 - Robinson, Simon A1 - Karst, Uwe A1 - Helmer, Rebecca A1 - Botnar, Rene A1 - Hamm, Bernd A1 - Makowski, Marcus Richard A1 - Brangsch, Julia T1 - Elastin-specific MR probe for visualization and evaluation of an interleukin-1β targeted therapy for atherosclerosis N2 - Atherosclerosis is a chronic inflammatory condition of the arteries and represents the primary cause of various cardiovascular diseases. Despite ongoing progress, finding effective anti-inflammatory therapeutic strategies for atherosclerosis remains a challenge. Here, we assessed the potential of molecular magnetic resonance imaging (MRI) to visualize the effects of 01BSUR, an anti-interleukin-1β monoclonal antibody, for treating atherosclerosis in a murine model. Male apolipoprotein E-deficient mice were divided into a therapy group (01BSUR, 2 × 0.3 mg/kg subcutaneously, n = 10) and control group (no treatment, n = 10) and received a high-fat diet for eight weeks. The plaque burden was assessed using an elastin-targeted gadolinium-based contrast probe (0.2 mmol/kg intravenously) on a 3 T MRI scanner. T1-weighted imaging showed a significantly lower contrast-to-noise (CNR) ratio in the 01BSUR group (pre: 3.93042664; post: 8.4007067) compared to the control group (pre: 3.70679168; post: 13.2982156) following administration of the elastin-specific MRI probe (p < 0.05). Histological examinations demonstrated a significant reduction in plaque size (p < 0.05) and a significant decrease in plaque elastin content (p < 0.05) in the treatment group compared to control animals. This study demonstrated that 01BSUR hinders the progression of atherosclerosis in a mouse model. Using an elastin-targeted MRI probe, we could quantify these therapeutic effects in MRI. N2 - Atherosklerose ist eine chronische entzündliche Erkrankung der Arterien und die Hauptursache für verschiedene Herz-Kreislauf-Erkrankungen. Trotz kontinuierlicher Fortschritte ist es nach wie vor schwierig, wirksame entzündungshemmende Therapiestrategien für Atherosklerose zu finden. In dieser Studie haben wir das Potenzial der molekularen Magnetresonanztomographie (MRT) zur Visualisierung der Wirkung von 01BSUR, einem monoklonalen Anti-Interleukin-1β-Antikörper, zur Behandlung von Atherosklerose in einem Mausmodell untersucht. Männliche Apolipoprotein-E-defiziente Mäuse wurden in eine Therapiegruppe (01BSUR, 2 × 0,3 mg/kg subkutan, n = 10) und eine Kontrollgruppe (keine Behandlung, n = 10) aufgeteilt und erhielten acht Wochen lang eine fettreiche Diät. Die Plaquebelastung wurde mit einer auf Elastin ausgerichteten Kontrastmittelsonde auf Gadoliniumbasis (0,2 mmol/kg intravenös) auf einem 3-T-MRT-Scanner untersucht. Die T1-gewichtete Bildgebung zeigte ein signifikant niedrigeres Kontrast-Rausch-Verhältnis (CNR) in der 01BSUR-Gruppe (vorher: 3,93042664; nachher: 8,4007067) im Vergleich zur Kontrollgruppe (vorher: 3,70679168; nachher: 13,2982156) nach Verabreichung der Elastin-spezifischen MRT-Sonde (p < 0,05). Histologische Untersuchungen zeigten eine signifikante Verringerung der Plaque-Größe (p < 0,05) und eine signifikante Abnahme des Plaque-Elastin-Gehalts (p < 0,05) in der Behandlungsgruppe im Vergleich zu den Kontrolltieren. Diese Studie zeigte, dass 01BSUR das Fortschreiten der Atherosklerose in einem Mausmodell hemmt. Mit einer auf Elastin ausgerichteten MRT-Sonde konnten wir diese therapeutischen Effekte in der MRT quantifizieren. KW - Atherosclerosis KW - Molecular imaging KW - Elastin KW - Plaque KW - Interleukin-1beta PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610858 DO - https://doi.org/10.1038/s41598-024-71716-5 VL - 14 IS - 1 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-61085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nerger, Tino A1 - Neumann, Patrick P. A1 - Weller, Michael G. T1 - Drone-Based Localization of Hazardous Chemicals by Passive Smart Dust N2 - The distribution of tiny sensors over a specific area was first proposed in the late 1990s as a concept known as smart dust. Several efforts focused primarily on computing and networking capabilities, but quickly ran into problems related to power supply, cost, data transmission, and environmental pollution. To overcome these limitations, we propose using paper-based (confetti-like) chemosensors that exploit the inherent selectivity of chemical reagents, such as colorimetric indicators. In this work, cheap and biodegradable passive sensors made from cellulose could successfully indicate the presence of hazardous chemicals, e.g., strong acids, by a significant color change. A conventional color digital camera attached to a drone could easily detect this from a safe distance. The collected data were processed to define the hazardous area. Our work presents a combination of the smart dust concept, chemosensing, paper-based sensor technology, and low-cost drones for flexible, sensitive, economical, and rapid detection of hazardous chemicals in high-risk scenarios. KW - Cellulose KW - Passive Smart Dust KW - Drohne KW - Kolorimetrische Sensoren PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614641 DO - https://doi.org/10.3390/s24196195 VL - 24 IS - 19 SP - 1 EP - 16 PB - MDPI AN - OPUS4-61464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tscheuschner, Georg A1 - Ponader, Marco A1 - Raab, Christopher A1 - Weider, Prisca S. A1 - Hartfiel, Reni A1 - Kaufmann, Jan Ole A1 - Völzke, Jule L. A1 - Bosc-Bierne, Gaby A1 - Prinz, Carsten A1 - Schwaar, T. A1 - Andrle, Paul A1 - Bäßler, Henriette A1 - Nguyen, Khoa A1 - Zhu, Y. A1 - Mey, A. S. J. S. A1 - Mostafa, A. A1 - Bald, I. A1 - Weller, Michael G. T1 - Efficient Purification of Cowpea Chlorotic Mottle Virus by a Novel Peptide Aptamer N2 - The cowpea chlorotic mottle virus (CCMV) is a plant virus explored as a nanotechnological platform. The robust self-assembly mechanism of its capsid protein allows for drug encapsulation and targeted delivery. Additionally, the capsid nanoparticle can be used as a programmable platform to display different molecular moieties. In view of future applications, efficient production and purification of plant viruses are key steps. In established protocols, the need for ultracentrifugation is a significant limitation due to cost, difficult scalability, and safety issues. In addition, the purity of the final virus isolate often remains unclear. Here, an advanced protocol for the purification of the CCMV from infected plant tissue was developed, focusing on efficiency, economy, and final purity. The protocol involves precipitation with PEG 8000, followed by affinity extraction using a novel peptide aptamer. The efficiency of the protocol was validated using size exclusion chromatography, MALDI-TOF mass spectrometry, reversed-phase HPLC, and sandwich immunoassay. Furthermore, it was demonstrated that the final eluate of the affinity column is of exceptional purity (98.4%) determined by HPLC and detection at 220 nm. The scale-up of our proposed method seems to be straightforward, which opens the way to the large-scale production of such nanomaterials. This highly improved protocol may facilitate the use and implementation of plant viruses as nanotechnological platforms for in vitro and in vivo applications. N2 - Das Cowpea Chlorotic Mottle Virus (CCMV) ist ein Pflanzenvirus, das als nanotechnologische Plattform erforscht wird. Der robuste Selbstorganisationsmechanismus seines Kapsidproteins ermöglicht die Verkapselung und gezielte Abgabe von Medikamenten. Darüber hinaus kann das Kapsid-Nanopartikel als programmierbare Plattform für die Präsentation verschiedener molekularer Komponenten verwendet werden. Im Hinblick auf künftige Anwendungen ist eine effiziente Produktion und Reinigung von Pflanzenviren von entscheidender Bedeutung. In etablierten Protokollen stellt die notwendige Ultrazentrifugation aufgrund von Kosten, schwieriger Skalierbarkeit und Sicherheitsaspekten eine erhebliche Einschränkung dar. Darüber hinaus bleibt die Reinheit des endgültigen Virusisolats oft unklar. Hier wurde ein fortschrittliches Protokoll für die Reinigung von CCMV aus infiziertem Pflanzengewebe entwickelt, wobei der Schwerpunkt auf Effizienz, Wirtschaftlichkeit und Reinheit lag. Das Protokoll beinhaltet eine Fällung mit Polyethylenglycol (PEG 8000), gefolgt von einer Affinitätsextraktion mit einem neuartigen Peptid-Aptamer. Die Effizienz des Protokolls wurde mithilfe von Größenausschluss-Chromatographie (SEC), MALDI-TOF-Massenspektrometrie, Umkehrphasen-HPLC und Sandwich-Immunoassay validiert. Darüber hinaus wurde nachgewiesen, dass das endgültige Eluat der Affinitätssäule eine außergewöhnliche Reinheit (98,4 %) aufweist, die durch HPLC und Detektion bei 220 nm bestimmt wurde. Die Skalierung der von uns vorgeschlagenen Methode scheint einfach zu sein, was den Weg für eine größer angelegte Produktion solcher Nanomaterialien ebnet. Dieses stark verbesserte Protokoll könnte die Verwendung und Umsetzung von Pflanzenviren als nanotechnologische Plattformen für In-vitro- und In-vivo-Anwendungen erleichtern. KW - Affinity chromatography KW - Nanoparticles KW - Nanoscience KW - Carrier protein KW - Encapsulation KW - Combinatorial peptide library KW - Peptide binder KW - Vigna unguiculata KW - Augenbohne KW - Schlangenbohne KW - Pflanzenvirus KW - Plant virus KW - Upscaling KW - Commercialization KW - Reference material KW - Nanocarrier PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572645 DO - https://doi.org/10.3390/v15030697 VL - 15 IS - 3 SP - 1 EP - 24 PB - MDPI CY - Basel, Schweiz AN - OPUS4-57264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beslic, D. A1 - Tscheuschner, Georg A1 - Renard, B. Y. A1 - Weller, Michael G. A1 - Muth, Thilo T1 - Comprehensive evaluation of peptide de novo sequencing tools for monoclonal antibody assembly N2 - Monoclonal antibodies are biotechnologically produced proteins with various applications in research, therapeutics and diagnostics. Their ability to recognize and bind to specific molecule structures makes them essential research tools and therapeutic agents. Sequence information of antibodies is helpful for understanding antibody–antigen interactions and ensuring their affinity and specificity. De novo protein sequencing based on mass spectrometry is a valuable method to obtain the amino acid sequence of peptides and proteins without a priori knowledge. In this study, we evaluated six recently developed de novo peptide sequencing algorithms (Novor, pNovo 3, DeepNovo, SMSNet, PointNovo and Casanovo), which were not specifically designed for antibody data. We validated their ability to identify and assemble antibody sequences on three multi-enzymatic data sets. The deep learning-based tools Casanovo and PointNovo showed an increased peptide recall across different enzymes and data sets compared with spectrum-graph-based approaches. We evaluated different error types of de novo peptide sequencing tools and their performance for different numbers of missing cleavage sites, noisy spectra and peptides of various lengths. We achieved a sequence coverage of 97.69–99.53% on the light chains of three different antibody data sets using the de Bruijn assembler ALPS and the predictions from Casanovo. However, low sequence coverage and accuracy on the heavy chains demonstrate that complete de novo protein sequencing remains a challenging issue in proteomics that requires improved de novo error correction, alternative digestion strategies and hybrid approaches such as homology search to achieve high accuracy on long protein sequences. KW - De novo peptide sequencing KW - Bioinformatics KW - Benchmarking study KW - Monoclonal antibody KW - Mass spectrometry KW - Sequence coverage KW - Light chains KW - Heavy chains KW - IgG KW - Immunoglobulins KW - Error correction KW - Sequencing algorithm KW - Preprocessing KW - Missing fragmentation sites KW - Deep learning-based tools PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570363 DO - https://doi.org/10.1093/bib/bbac542 VL - 24 IS - 1 SP - 1 EP - 12 PB - Oxford University Press AN - OPUS4-57036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fröhlich-Nowoisky, J. A1 - Bothen, N. A1 - Backes, A. T. A1 - Weller, Michael G. A1 - Pöschl, U. T1 - Oligomerization and tyrosine nitration enhance the allergenic potential of the birch and grass pollen allergens Bet v 1 and Phl p 5 N2 - Protein modifications such as oligomerization and tyrosine nitration alter the immune response to allergens and may contribute to the increasing prevalence of allergic diseases. In this mini-review, we summarize and discuss relevant findings for the major birch and grass pollen allergens Bet v 1 and Phl p 5 modified with tetranitromethane (laboratory studies), peroxynitrite (physiological processes), and ozone and nitrogen dioxide environmental conditions). We focus on tyrosine nitration and the formation of protein dimers and higher oligomers via dityrosine cross-linking and the immunological effects studied. N2 - Proteinmodifikationen wie Oligomerisierung und Tyrosinnitrierung verändern die Immunantwort auf Allergene und tragen möglicherweise zur zunehmenden Prävalenz allergischer Erkrankungen bei. In diesem Mini-Review fassen wir relevante Befunde zu den wichtigsten Birken- und Gräserpollenallergenen Bet v 1 und Phl p 5 zusammen, die mit Tetranitromethan (Laborstudien), Peroxynitrit (physiologische Prozesse) und Ozon und Stickstoffdioxid (Umweltbedingungen). Wir konzentrieren uns auf die Tyrosin-Nitrierung und die Bildung von Proteindimeren und höheren Oligomeren durch Dityrosin-Vernetzung und deren immunologischen Auswirkungen. KW - Allergy KW - Nitration KW - Protein oligomers KW - Air pollution KW - Ozone KW - Nitrogen oxides KW - Tyrosine KW - Nitrotyrosine KW - Dityrosine KW - Dityrosine crosslinking KW - Protein degradation KW - Neoepitopes KW - Neoallergen KW - IgE KW - Immunoglobulin E PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591453 DO - https://doi.org/10.3389/falgy.2023.1303943 VL - 4 SP - 1 EP - 8 PB - Frontiers Media CY - Switzerland AN - OPUS4-59145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinmuth-Selzle, K. A1 - Bellinghausen, I. A1 - Leifke, A. L. A1 - Backes, A. T. A1 - Bothen, N. A1 - Ziegler, K. A1 - Weller, Michael G. A1 - Saloga, J. A1 - Schuppan, D. A1 - Lucas, K. A1 - Pöschl, U. A1 - Fröhlich-Nowoisky, J. T1 - Chemical modification by peroxynitrite enhances TLR4 activation of the grass pollen allergen Phl p 5 N2 - The chemical modification of aeroallergens by reactive oxygen and nitrogen species (ROS/RNS) may contribute to the growing prevalence of respiratory allergies in industrialized countries. Post-translational modifications can alter the immunological properties of proteins, but the underlying mechanisms and effects are not well understood. In this study, we investigate the Toll-like receptor 4 (TLR4) activation of the major birch and grass pollen allergens Bet v 1 and Phl p 5, and how the physiological oxidant peroxynitrite (ONOO–) changes the TLR4 activation through protein nitration and the formation of protein dimers and higher oligomers. Of the two allergens, Bet v 1 exhibited no TLR4 activation, but we found TLR4 activation of Phl p 5, which increased after modification with ONOO– and may play a role in the sensitization against this grass pollen allergen. We attribute the TLR4 activation mainly to the two-domain structure of Phl p 5 which may promote TLR4 dimerization and activation. The enhanced TLR4 signaling of the modified allergen indicates that the ONOO–-induced modifications affect relevant protein-receptor interactions. This may lead to increased sensitization to the grass pollen allergen and thus contribute to the increasing prevalence of allergies in the Anthropocene, the present era of globally pervasive anthropogenic influence on the environment. KW - Bet v 1 KW - Birch pollen allergen KW - Phl p 5 KW - Grass pollen KW - Phleum pratense KW - Betula pendula KW - Nitration KW - Nitrotyrosine KW - Protein nitration KW - Toll-like receptor 4 KW - Allergy KW - Enhancement KW - Oligomerization KW - Dimerization KW - TLR4 activation KW - Air pollution KW - Nitrogen oxides KW - Inflammation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570298 DO - https://doi.org/10.3389/falgy.2023.1066392 VL - 4 SP - 1 EP - 7 PB - Frontiers Media SA CY - Lausanne, Switzerland AN - OPUS4-57029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tchipilov, Teodor A1 - Meyer, Klas A1 - Weller, Michael G. T1 - Quantitative 1H nuclear magnetic resonance (qNMR) of aromatic amino acids for protein quantification N2 - Hydrolysis of protein samples into amino acids facilitates the use of NMR spectroscopy for protein and peptide quantification. Different conditions have been tested for quantifying aromatic amino acids and proteins. The pH-dependent signal shifts in the aromatic region of amino acid samples were examined. A pH of 12 was found to minimize signal overlap of the four aromatic amino acids. Several aromatic compounds, such as terephthalic acid, sulfoisophthalic acid, and benzene tricarboxylic acid, were applied as internal standards. The quantification of amino acids from an amino acid standard was performed. Using the first two suggested internal standards, recovery was ~97% for histidine, phenylalanine, and tyrosine at a concentration of approximately 1 mM in solution. Acidic hydrolysis of a certified reference material (CRM) of bovine serum albumin (BSA) and subsequent quantification of Phe and Tyr yielded recoveries of 98% ± 2% and 88% ± 4%, respectively, at a protein concentration of 16 g/L or 250 µM. KW - Amino acid analysis KW - Aromatic amino acid analysis KW - AAA KW - AAAA KW - Protein hydrolysis KW - Hydrochloric acid KW - Metrology KW - Traceability KW - NIST KW - Reference materials KW - Internal standard KW - Calibration KW - Compound-independent calibration KW - Histidine KW - Tyrosine KW - Tryptophan KW - Phenylalanine KW - Terephthalic acid KW - Benzene-1,3,5-tricarboxylic acid KW - Bovine serum albumin (BSA) KW - Quantitative protein analysis KW - Phenylketonuria PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570943 DO - https://doi.org/10.3390/mps6010011 VL - 6 IS - 1 SP - 1 EP - 13 PB - MDPI CY - Basel, Schweiz AN - OPUS4-57094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, Yanchen A1 - de Oliveira Guilherme Buzanich, Ana A1 - Montoro, Luciano A. A1 - Liu, Hao A1 - Liu, Ye A1 - Emmerling, Franziska A1 - Russo, Patrícia A. A1 - Pinna, Nicola T1 - A partially disordered crystallographic shear block structure as fast-charging negative electrode material for lithium-ion batteries N2 - A well-ordered crystalline structure is crucial in battery electrodes, as the dimensionality and connectivity of the interstitial sites inherently influence Li+ ions diffusion kinetics. Niobium tungsten oxides block structures, composed of ReO3-type blocks of specific sizes with well-defined metal sites, are promising fast-charging negative electrode materials. Structural disorder is generally detrimental to conductivity or ion transport. However, here, we report an anomalous partially disordered Nb12WO33 structure that significantly enhances Li-ion storage performance compared to the known monoclinic Nb12WO33 phase. The partially disordered phase consists of corner-shared NbO6 octahedra blocks of varied sizes, including 5×4, 4×4, and 4×3, with a disordered arrangement of distorted WO4 tetrahedra at the corners of the blocks. This structural arrangement is robust during lithiation/delithiation, exhibiting minor local structure changes during cycling. It enables accelerated Li-ion migration, resulting in promising fast-charging performance, namely, 62.5 % and 44.7 % capacity retention at 20 C and 80 C, respectively. This study highlights the benefits of introducing disorder into niobium tungsten oxide shear structures, through the establishment of clear structure-performance correlations, offering guidelines for designing materials with targeted properties. KW - Lithium ion batteries KW - Oxides KW - XANES KW - XRD PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637994 DO - https://doi.org/10.1038/s41467-025-61646-9 SN - 2041-1723 VL - 16 IS - 1 SP - 1 EP - 15 PB - Springer Science and Business Media LLC AN - OPUS4-63799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinekamp, Christian A1 - Roy, Arkendu A1 - Karafiludis, Stephanos A1 - Kumar, Sourabh A1 - de Oliveira Guilherme Buzanich, Ana A1 - Stawski, Tomasz M. A1 - Miliūtė, Aistė A1 - von der Au, Marcus A1 - Ahrens, Mike A1 - Braun, Thomas A1 - Emmerling, Franziska T1 - Zirconium fluoride-supported high-entropy fluoride: a catalyst for enhanced oxygen evolution reaction N2 - Extended hydrogen initiatives promote the urgency of research on water splitting technologies and, therein, oxygen evolution reaction catalysts being developed. A route to access a ZrF4 supported high-entropy fluoride catalyst using a facile sol–gel route is presented. The high-entropy character of the catalyst was confirmed by scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDX) as well as inductively coupled plasma-mass spectrometry (ICP-MS). Additional investigations on the local structure were performed using extended X-ray absorption fine structure spectroscopy (EXAFS) and pair distribution function (PDF) analysis. The catalyst shows significant potential for oxygen evolution reaction (OER) in alkaline media with a current density of 100 mA cm−2 at approximately 1.60 V, thus outperforming benchmark materials such as IrO2, despite a significant reduction in electrochemical mass loading. A potential mechanism is suggested based on free energy calculation using DFT calculations. KW - OER KW - HEA KW - CCMAT PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637116 DO - https://doi.org/10.1039/D4TA08664C SN - 2050-7488 VL - 13 IS - 26 SP - 20383 EP - 20393 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmar, Stefan A1 - Weyrauch, Steffen A1 - Reemtsma, Thorsten A1 - Eisentraut, Paul A1 - Altmann, Korinna A1 - Ruhl, Aki S. A1 - Jekel, Martin T1 - Settling Velocities of Tire and Road Wear Particles: Analyzing Finely Graded Density Fractions of Samples from a Road Simulator and a Highway Tunnel N2 - The terminal settling velocity is considered the most critical parameter determining the transport of tire and road wear particles (TRWP) in aquatic environments. Nonetheless, no respective empirical data has been reported so far. In this study, particle samples from a road simulator and a highway tunnel were investigated with a validated imaging method. Different density and size fractions of both samples were measured separately, acquiring sizes and settling velocities of more than 30,000 individual particles. In addition, tire marker polymers were analyzed for each fraction via thermal extraction desorption-gas chromatography/mass spectrometry. Finally, the acquired particle data was combined according to the fractions’ estimated tire contents in order to deduce detailed probability distributions of particle size and settling velocity for the actual TRWP from both samples. Weighted by TRWP-incorporated tire mass, median diameters of 54 and 44 μm as well as median settling velocities of 0.65 and 0.22 mm/s were found for TRWP from the road simulator and highway tunnel, respectively. This study thus provides the first ever empirical data on TRWP settling velocities in water, which can be highly valuable input for modeling the environmental transport of TRWP and for dimensioning TRWP retention systems. KW - Microplastics KW - TED-GC/MS KW - Sinking velocities KW - Transport PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635449 DO - https://doi.org/10.1021/acs.est.5c04165 SN - 0013-936X VL - 59 IS - 26 SP - 13434 EP - 13446 PB - American Chemical Society (ACS) AN - OPUS4-63544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Das, Prasenjit A1 - Chakraborty, Gouri A1 - Yang, Jin A1 - Roeser, Jérôme A1 - Küçükkeçeci, Hüseyin A1 - Nguyen, Anh Dung A1 - Schwarze, Michael A1 - Gabriel, Jose A1 - Penschke, Christopher A1 - Du, Shengjun A1 - Weigelt, Vincent A1 - Khalil, Islam E. A1 - Schmidt, Johannes A1 - Saalfrank, Peter A1 - Oschatz, Martin A1 - Rabeah, Jabor A1 - Schomäcker, Reinhard A1 - Emmerling, Franziska A1 - Thomas, Arne T1 - The Effect of Pore Functionality in Multicomponent Covalent Organic Frameworks on Stable Long‐Term Photocatalytic H2 Production N2 - AbstractIn nature, organic molecules play a vital role in light harvesting and photosynthesis. However, regarding artificial water splitting, the research focus is primarily on inorganic semiconductors. Although organic photocatalysts have high structural variability, they tend to exhibit lower quantum efficiencies for water splitting than their inorganic counterparts. Multicomponent reactions (MCRs) offer an attractive route to introduce different functional units into covalent organic frameworks (COFs) and enable semiconducting properties and high chemical stability, creating promising materials for long‐term photocatalytic applications, such as H2 production. Herein, five highly crystalline donor‐acceptor based, 4‐substituted quinoline‐linked MCR‐COFs are presented that are prepared via the three‐component Povarov reaction. The pore functionality is varied by applying different vinyl derivatives (e.g., styrene, 2‐vinyl pyridine, 4‐vinylpyridine, 4‐vinyl imidazole, 2,3,4,5,6‐pentafluorostyrene), which has a strong influence on the obtained photocatalytic activity. Especially an imidazole‐functionalized COF displays promising photocatalytic performance due to its high surface area, crystallinity, and wettability. These properties enable it to maintain its photocatalytic activity even in a membrane support. Furthermore, such MCR‐COFs display dramatically enhanced (photo)chemical stability even after long‐term solar light irradiation and exhibit a high and steady H2 evolution for at least 15 days. KW - Sstability KW - Covalent organic frameworks KW - Pore functionality KW - Long-term H2 production KW - Multicomponent reactions PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639787 DO - https://doi.org/10.1002/aenm.202501193 SN - 1614-6832 SP - 1 EP - 10 PB - Wiley VHC-Verlag AN - OPUS4-63978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Visileanu, Emilia A1 - Altmann, Korinna A1 - Stepa, Raluca A1 - Haiducu, Maria A1 - Miclea, Paul Tiberiu A1 - Vladu, Alina A1 - Dondea, Felicia A1 - Grosu, Marian Catalin A1 - Scarlat, Razvan T1 - Comparative Analysis of Airborne Particle Concentrations in Textile Industry Environments Throughout the Workday N2 - This paper addresses the growing concern surrounding microplastic pollution, particularly within the textile industry, and the associated potential health risks linked to the inhalation and ingestion of microplastic particles. Microplastics, defined as plastic particles smaller than five millimeters, are increasingly found not only in aquatic environments, but also in soils, air, and food. Although research on the health impacts of microplastics is still emerging, early studies indicate that these particles could contribute to health issues, including oxidative stress, inflammation, and cardiovascular diseases. Notably, individuals with higher concentrations of plastics in arterial plaques are more susceptible to heart attacks and strokes. In the textile industry, synthetic fibers such as polyester, nylon, and acrylic release microplastics into the air during production. The paper discusses a study conducted in a textile company that processes polyester yarns, where airborne microplastic concentrations were measured at various locations throughout the day. Particle sizes ranging from 0.3 nm to 10 nm were analyzed, revealing the presence of polyester polymers in the particulate matter. These findings underscore the widespread nature of microplastic pollution, particularly in industrial settings, and raise concerns about the health risks associated with prolonged exposure to airborne microplastics. While further research is necessary to fully understand the extent of these health impacts, preliminary data suggest a troubling link between microplastic inhalation and cardiovascular conditions. KW - Microplastics KW - Textiles KW - Airborne particles PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635269 DO - https://doi.org/10.3390/microplastics4020034 SN - 2673-8929 VL - 4 IS - 2 SP - 1 EP - 17 PB - MDPI AG AN - OPUS4-63526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodríguez-Sánchez, Noelia A1 - Domínguez-Santos, J. Enrique A1 - Bhattacharya, Biswajit A1 - Prinz, Carsten A1 - Canosa, Inés A1 - Flores, Amando A1 - Jiménez-Rodríguez, Antonia A1 - Ruiz-Salvador, A. Rabdel A1 - Emmerling, Franziska A1 - Ballesteros, Menta T1 - Mechanochemical synthesis of multivariate UPO-3 (Cu-ZIF-9-ica) MOF for inactivation of antibiotic-resistant bacteria and irrigation-quality water production via heterogeneous photo-Fenton catalysis N2 - Water scarcity and pollution are critical global challenges, particularly in agriculture, the largest consumer of water. The development of sustainable, effective, and environmentally friendly disinfection methods is essential to address the risks posed by antibiotic-resistant bacteria and to ensure safe reuse of water for irrigation. In this study, we report the synthesis of the metal-organic framework (MOF) Universidad Pablo de Olavide-3 (UPO-3) via a mechanochemical approach, a scalable and sustainable method compared to traditional solvothermal synthesis. The resulting UPO-3/H2O2 system exhibits robust photocatalytic properties under visible light, achieving effective and broad-spectrum antibacterial activity. The disinfection efficiency of the catalyst was evaluated against Escherichia coli as a model of microbial pathogen in two saline matrices, considering the key parameters of the heterogeneous photo-Fenton process, including catalyst dosage, initial H2O2 concentration, and light irradiation. Notably, it inactivated two important virulent and antibiotic-resistant bacterial pathogens (Staphylococcus aureus and Pseudomonas aeruginosa). Furthermore, UPO-3 shows exceptional performance under real-world conditions, such as river water disinfection, achieving >5-log reduction of E. coli, fulfilling a critical criterion for Class A water reuse under Regulation (EU) 2020/741. These results highlight UPO-3 as a versatile and sustainable solution for water reuse, addressing water scarcity and advancing efforts to achieve United Nations Sustainable Development Goal 6. KW - Water reuse KW - Antibiotic-resistant bacteria KW - Water disinfection KW - Mechanochemical synthesis KW - Metal organic framework PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639766 DO - https://doi.org/10.1016/j.chemosphere.2025.144610 SN - 0045-6535 VL - 386 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-63976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Go, Eun Sul A1 - Hong, Eun Ji A1 - Lee, Ji Yeong A1 - Stolar, Tomislav A1 - Peterson, Gregory I. A1 - Emmerling, Franziska A1 - Kim, Kyoungsoo A1 - Kim, Jeung Gon T1 - Insights into Mechanochemical Solid-State Ball-Milling Reaction: Monitoring Transition from Heterogeneous to Homogeneous Conditions N2 - As mechanochemical synthesis has advanced significantly, there has been intense interest in understanding the underlying mechanisms of these reactions. Given that many mechanochemical processes are conducted in the solid-state without solvation yet sometimes yield faster reactions than those in solution, we sought to address the following question: Are mechanochemical reactions homo- or heterogeneous? To investigate, we employed a model system involving the mixing and copolymerization of l-lactide (LLA) and d-lactide (DLA), monitored through powder X-ray diffraction (PXRD), nuclear magnetic resonance, and differential scanning calorimetry. In situ and ex situ PXRD analyses of the mixture of LLA and DLA showed that vibratory ball milling rapidly transformed the initially heterogeneous lactide mixture into a homogeneous phase within one min due to collisions between the balls and the jar. By varying the milling conditions, we were able to regulate the level of mixing, which subsequently influenced the copolymerization outcomes. In the solid-state ball-milling copolymerization of LLA and DLA in the presence of a catalyst and initiator, multiblock copolymers of poly(l-lactic acid) and poly(d-lactic acid) were formed within one min during the early stage of the reaction, when incomplete mixing of the monomers led to a process governed by phase heterogeneity. In contrast, prolonged polymerization promoted conditions approaching homogeneity, ultimately yielding atactic poly(lactic acid). This transition from heterogeneous to homogeneous reactions is a distinctive feature compared to conventional homogeneous reactions, potentially leading to mechano-exclusive reaction designs. KW - Mechanochemistry KW - Ball-milling KW - Homogeneous reaction KW - Heterogeneous reaction PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638008 DO - https://doi.org/10.1021/jacsau.5c00322 SN - 2691-3704 VL - 5 IS - 6 SP - 2720 EP - 2727 PB - American Chemical Society (ACS) AN - OPUS4-63800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -