TY - CONF A1 - Sander, Luise T1 - Linking material and electrode properties to the cell performance of commercially available sodium-ion cells N2 - As the first commercial sodium-ion-batteries (SIBs) are available for purchase, it is possible to investigate material composition. Gaining an insight into the material composition of these SIBs is of interest not only for the classification of possible safety risks and hazards, but also in regard to recycling. Herein we report the preliminary investigations of the chemical and structural composition of first commercial SIB-cells.[1,2] Two different SIB-cell types were compared in terms of electrode size, thickness, loading etc. Furthermore, the composition of the active materials and electrolyte was investigated and compared. Finally, the gained results were linked to the different data sheet performance of the two cell types. T2 - Batterieforum Deutschland 2026 CY - Berlin, Germany DA - 20.01.2026 KW - Electrochemical Energy Storage KW - Battery KW - Sodium-ion-battery KW - EES KW - Energy Storage PY - 2026 AN - OPUS4-65588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eddah, Mustapha T1 - Multi-Energy High Dynamic Range (HDR) Synchrotron X-ray Computed Tomography applied to LTCC samples N2 - Synchrotron X-ray computed tomography (SXCT) is regularly used in materials science to correlate structural properties with macroscopic properties and to optimize manufacturing processes. The X-ray beam energy must be adapted to the sample properties, such as size and density. If both strongly and weakly absorbing materials are present, the contrast to the weakly absorbing materials is lost, resulting in image artifacts and a poor signal-to-noise ratio (SNR). One particular example is a low-temperature co-fired ceramics (LTCC), in which metal connections are embedded in a ceramic matrix and form 3-dimensional conducting structures. This article describes a method of combining SXCT scans acquired at different beam energies, significantly reducing metal artifacts, and improving image quality. We show how to solve the difficult task of merging the scans at low and high beam energy. Our proposed merging approach achieves up to 35 % improvement in SNR within ceramic regions adjacent to metallic conductors. In this way, previously inaccessible regions within the ceramic structure close to the metallic conductors are made accessible. T2 - iCT 2026 CY - Linz, Austria DA - 10.02.2026 KW - Synchrotron x-ray CT KW - Reconstruction algorithm KW - Low-Temperature cofired ceramics KW - Data merging PY - 2026 AN - OPUS4-65583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Diana A1 - Hahn, Oliver T1 - Colours on Maps - Purpose and Materiality N2 - Colours are an inseparable attribute of most maps. While colouring seems at first glance simply superficial ‘prettifying’ of maps, most maps were given colours for other reasons: colour is an important key to understanding the function and use of maps. The use of colours, the choice of where to assign them and the meaning given to them has accordingly never been static but has changed over time. In this context, the three aspects: colour system, colour scheme, and colour code are of particular importance. Material scientific analysis makes it possible to find out more about the material composition of colourants (pigments and dyes) on maps. The study of colourants provides insights into the production conditions and use of maps. Furthermore, it offers clues about colour changes and forms the basis for appropriate restoration concepts. T2 - Maps. Digital. Analogue CY - Oxford, United Kingdom of Great Britain and Northern Ireland DA - 26.02.2026 KW - Maps KW - Colours KW - Archaeometry KW - Aging PY - 2026 AN - OPUS4-65599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eddah, Mustapha T1 - Multi-Energy High Dynamic Range (HDR) Synchrotron X-ray Computed Tomography applied to LTCC samples N2 - Synchrotron X-ray computed tomography (SXCT) is regularly used in materials science to correlate structural properties with macroscopic properties and to optimize manufacturing processes. The X-ray beam energy must be adapted to the sample properties, such as size and density. If both strongly and weakly absorbing materials are present, the contrast to the weakly absorbing materials is lost, resulting in image artifacts and a poor signal-to-noise ratio (SNR). One example is a low-temperature co-fired ceramics (LTCC), in which metal connections are embedded in a ceramic matrix and form 3-dimensional conducting structures. This article describes a method of combining SXCT scans acquired at different beam energies, significantly reducing metal artifacts, and improving image quality. We show how to solve the difficult task of merging the scans at low and high beam energy. Our proposed merging approach achieves up to 35% improvement in SNR within ceramic regions adjacent to metallic conductors. In this way, previously inaccessible regions within the ceramic structure close to the metallic conductors are made accessible. T2 - iCT 2026 CY - Linz, Austria DA - 10.02.2026 KW - Synchrotron x-ray CT KW - Multi-energy CT KW - Low-Temperature cofired ceramics PY - 2026 AN - OPUS4-65586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino A1 - Neumann, Patrick P. A1 - Weller, Michael G. T1 - A New Approach: Passive Smart Dust for Detection of Hazardous Substances N2 - Remote sensing of hazardous substances is a key task that can be achieved with the help of remotely operated platforms equipped with specific sensors. A huge variety of methods and used vehicles have been developed for different purposes in recent years. The term smart dust refers to a science fiction novel and develop shortly after into a research proposal at UC Berkley funded by DARPA. Subsequently, the topic gained attraction but was overall considered as to complex for the technologies available at that time. In the launched passive smart dust project, we shift to a simple “chemical intelligent” passive sensor particle on the ground combined a read-out active sensor attached to an Unmanned Aerial Vehicle (UAV). The reactive particle surface can be preadjusted in the lab for exact desired properties regarding certain reactions to hazardous substances. Moreover, the aimed interaction with the active sensor can be modified. Planed applications allow for different materials e.g., for short time measurement, being ecologically degradable, or weather stable for long time monitoring. T2 - 38th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Poros, Greece DA - 20.09.2022 KW - Smart Dust KW - Drone KW - Remote Detection KW - Hazardous substances PY - 2022 SP - 1 EP - 2 CY - Athens, Greece AN - OPUS4-55925 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diepeveen, L. E. A1 - Laarakkers, C. M. M. A1 - Martos, G. A1 - Pawlak, M. E. A1 - Uguz, F. F. A1 - Verbene, K. E. S. A. A1 - van Swelm, R. P. L. A1 - Klaver, S. A1 - de Haan, A. F. J. A1 - Pitts, K. R. A1 - Bansal, S. S. A1 - Abbas, Ioana M. A1 - Fillet, M. A1 - Lefebvre, T. A1 - Geurts-Moespot, A. J. A1 - Girelli, D. A1 - Castagna, A. A1 - Herkert, M. A1 - Itkonen, O. A1 - Olbina, G. A1 - Tomosugi, N. A1 - Westerman, M. E. A1 - Delatour, V. A1 - Weykamp, C. W. A1 - Swinkels, D. W. T1 - Provisional standardization of hepcidin assays: creating a traceability chain with a primary reference material, candidate reference method and a commutable secondary reference material N2 - Hepcidin-25 concentrations measured by various methods differ considerably, complicating interpretation. Here, a previously identified plasma-based candidate secondary reference material (csRM) was modified into a serum-based two-leveled sRM. We validated its functionality to increase the equivalence between methods for international standardization. We applied technical procedures developed by the International Consortium for Harmonization of Clinical Laboratory Results. The sRM, consisting of lyophilized serum with cryolyoprotectant, appeared commutable among nine different measurement procedures using 16 native human serum samples in a first round robin (RR1). Harmonization potential of the sRM was simulated in RR1 and evaluated in practice in RR2 among 11 measurement procedures using three native human plasma samples. Comprehensive purity analysis of a candidate primary RM (cpRM) was performed by state-of-the-art procedures. The sRM was value assigned with an isotope dilution mass spectrometry-based candidate reference method calibrated using the certified pRM. The inter-assay CV without harmonization was 42.1% and 52.8% in RR1 and RR2, respectively. In RR1, simulation of harmonization with sRM resulted in an inter-assay CV of 11.0%, whereas in RR2 calibration with the material resulted in an inter-assay CV of 19.1%. Both the sRM and pRM passed international homogeneity criteria and showed long-term stability. We assigned values to the low (0.95 ± 0.11 nmol/L) and middle concentration (3.75 ± 0.17 nmol/L) calibrators of the sRM. Standardization of hepcidin is possible with our sRM, which value is assigned by a pRM. We propose the implementation of this material as an international calibrator for hepcidin-25. KW - Reference material KW - Peptide KW - Biomarker KW - Bioanalysis KW - Mass spectrometry KW - LC-MS/MS KW - Iron deficiency KW - MALDI-TOF MS KW - UHPLC-MS/MS KW - ELISA KW - Immunoassay PY - 2018 DO - https://doi.org/10.1515/cclm-2018-0783 SN - 1437-4331 SN - 1434-6621 VL - 57 IS - 6 SP - 864 EP - 872 PB - De Gruyter CY - Berlin AN - OPUS4-47153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Costa, Elena A1 - Climent Terol, Estela A1 - Ast, S. A1 - Weller, Michael G. A1 - Canning, J. A1 - Rurack, Knut T1 - Development of a lateral flow test for rapid pyrethroid detection using antibody-gated indicator-releasing hybrid materials N2 - The employment of type-I pyrethroids for airplane disinfection in recent years underlines the necessity to develop sensing schemes for the rapid detection of these pesticides directly at the point-of-use. Antibody-gated indicator-releasing materials were thus developed and implemented with test strips for lateral-flow assay-based analysis employing a smartphone for readout. Besides a proper matching of pore sizes and gating macromolecules, the functionalization of both the material's outer surface as well as the strips with PEG chains enhanced system performance. This simple assay allowed for the detection of permethrin as a target molecule at concentrations down to the lower ppb level in less than 5 minutes. KW - Lateral flow test KW - Gated hybrid material KW - Fluorescence KW - Smartphone readout device KW - Pyrethroid KW - Pesticide KW - Insecticide KW - SBA-15 KW - Permethrin PY - 2020 DO - https://doi.org/10.1039/d0an00319k SN - 0003-2654 SN - 1364-5528 VL - 145 IS - 10 SP - 3490 EP - 3494 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Climent Terol, Estela T1 - Antibody-gated indicator releasing mesoporous materials: a potential biosensor platform to be used in the development of rapid tests N2 - The urgent necessity to carry out reliable and relevant analytical measurements directly at a point-of-need is one of the current drivers for the development of miniaturised analytical systems, quick tests and wearables. Despite their simplicity, this type of tests must guarantee analytical relevance and reliability like laboratory-based analysis, e.g., in terms of sensitivity, selectivity, immunity against false positives and false negatives as well as robustness and repeatability. Keeping in mind the high sensitivity offered by gated indicator-releasing micro- and nanoparticles due to their inherent features of signal amplification, we performed several optimisations to develop a potential biosensor platform for use in rapid tests. Conceptually, these gated materials are closely related to drug delivery systems, consisting of high porous materials usually closed with macromolecular “caps” and loaded with indicator molecules that are released in presence of a target analyte. However, the key difference between the two types of functional materials is that many drug delivery systems should deliver their cargo over a longer period, often many hours, whereas the gated materials prepared for sensing should show fast release kinetics, on the order of <5 min. With the aim to optimise and adapt gated materials for sensing purposes, we prepared in this work several antibody-gated materials for small-molecule sensing. The materials consisted of porous silica particles containing indicator molecules in the pores and certain hapten molecules grafted to the particle surface close to the pore openings. The pores were then capped with antibodies binding to these haptens, thus inhibiting the escape of the indicators from inside of the pores. In presence of the corresponding analyte, the antibody is displaced from the surface of the material, allowing the escape of the indicators. This allows the detection of the analyte indirectly through an inherent signal amplification. In this work, the insecticide permethrin, a type-I pyrethroid, was selected as target model, because type-I pyrethroids play an important role in airplane disinfection. A first in-depth study of the various chemical tuning options of such antibody gated systems was performed. Different mesoporous silica supports, different functionalisation routes and different loading sequences were assessed. The materials’ performances were evaluated by studying their temporal response behaviour and detection sensitivity, including the tightness of pore closure (through the amount of blank release in absence of analyte) and the release kinetics. Our results indicate that the better the paratope-accommodating Fab region of the antibody “cap” fits into the host material’s pore openings, the better the closing/opening mechanism can be controlled. Because such materials can be used in various different formats from suspension assays[1] via microfluidic chips[2] to test strip-based lateral flow assays,[3] such materials present a powerful analytical particle platform for the sensitive analytics and diagnostics outside of a laboratory, realising sensitivities down to the µg kg–1 range in less analysis times of less than 5 min as we have recently demonstrated.[4] T2 - Biosensors for Pandemics CY - Online conference DA - 06.05.2020 KW - Hybrid materials KW - Pyrethroids KW - Signal amplification PY - 2020 UR - http://www.confstreaming.com/Biosensors2020/ AN - OPUS4-50746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Climent Terol, Estela T1 - Antibody-gated indicator releasing mesoporous materials: a potential biosensor platform to be used in the development of rapid tests N2 - The urgent necessity to carry out reliable and relevant analytical measurements directly at a point-of-need is one of the current drivers for the development of miniaturised analytical systems, quick tests and wearables. Despite their simplicity, this type of tests must guarantee analytical relevance and reliability like laboratory-based analysis, e.g., in terms of sensitivity, selectivity, immunity against false positives and false negatives as well as robustness and repeatability. Keeping in mind the high sensitivity offered by gated indicator-releasing micro- and nanoparticles due to their inherent features of signal amplification, we performed several optimisations to develop a potential biosensor platform for use in rapid tests. Conceptually, these gated materials are closely related to drug delivery systems, consisting of high porous materials usually closed with macromolecular “caps” and loaded with indicator molecules that are released in presence of a target analyte. However, the key difference between the two types of functional materials is that many drug delivery systems should deliver their cargo over a longer period, often many hours, whereas the gated materials prepared for sensing should show fast release kinetics, on the order of <5 min. With the aim to optimise and adapt gated materials for sensing purposes, we prepared in this work several antibody-gated materials for small-molecule sensing. The materials consisted of porous silica particles containing indicator molecules in the pores and certain hapten molecules grafted to the particle surface close to the pore openings. The pores were then capped with antibodies binding to these haptens, thus inhibiting the escape of the indicators from inside of the pores. In presence of the corresponding analyte, the antibody is displaced from the surface of the material, allowing the escape of the indicators. This allows the detection of the analyte indirectly through an inherent signal amplification. In this work, the insecticide permethrin, a type-I pyrethroid, was selected as target model, because type-I pyrethroids play an important role in airplane disinfection. A first in-depth study of the various chemical tuning options of such antibody gated systems was performed. Different mesoporous silica supports, different functionalisation routes and different loading sequences were assessed. The materials’ performances were evaluated by studying their temporal response behaviour and detection sensitivity, including the tightness of pore closure (through the amount of blank release in absence of analyte) and the release kinetics. Our results indicate that the better the paratope-accommodating Fab region of the antibody “cap” fits into the host material’s pore openings, the better the closing/opening mechanism can be controlled. Because such materials can be used in various different formats from suspension assays[1] via microfluidic chips[2] to test strip-based lateral flow assays,[3] such materials present a powerful analytical particle platform for the sensitive analytics and diagnostics outside of a laboratory, realising sensitivities down to the µg kg–1 range in less analysis times of less than 5 min as we have recently demonstrated.[4] T2 - Biosensors for Pandemics CY - Online conference DA - 06.05.2020 KW - Hybrid materials KW - Pyrethroids KW - Signal amplification PY - 2020 UR - http://www.confstreaming.com/Biosensors2020/ AN - OPUS4-50744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völzke, Jule L. T1 - Immunoprecipitation with Nanodiamonds for the Enrichment of Ceruloplasmin from Human Serum N2 - In this study, we developed a new immunoprecipitation method based on protein-coated nanodiamonds. Performing SDS-PAGE and using the SDS-PAGE buffer as an eluent showed that CER could be successfully enriched from human serum. Based on the copper determination with ICP-MS, the amount of bound CER on the nanodiamonds can be calculated. We could show the fulfilled mass balance of bound CER and CER in the supernatant after incubation with a known amount of CER. For isotope ratio analysis this method can be applied to compare ratios of the total copper content in human serum to copper ratios from CER enrichment. T2 - ReMiND 2019 CY - Braunschweig, Germany DA - 26.06.2019 KW - Metalloprotein KW - Copper KW - Affinity enrichment KW - Immunoaffinity KW - Protein g KW - Blood KW - Serum KW - Plasma KW - SDS-PAGE KW - ICP-MS PY - 2019 UR - https://www.ptb.de/empir/remind-conference.html AN - OPUS4-49728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Costa, Elena T1 - Development of a lateral flow test for rapid pyrethroid detection N2 - Type-I pyrethroids are frequently used for disinfection purposes on airplanes from and to tropical areas as a preventive health measure to control or kill the insect vectors of human diseases including dengue, yellow fever and malaria. The aim of the presented work was the development of such a simple, rapid and effective method for pyrethroid analysis T2 - Biosensors2020 CY - Online meeting DA - 06.05.2020 KW - Nomaterials KW - Lateral flow test KW - Pyrethroids KW - Antibodies KW - Gated delivery systems KW - Biosensors PY - 2020 AN - OPUS4-50755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Fischer, Janina T1 - Suspensionsarray-Fluoreszenzimmunoassay zur Multiplexbestimmung von SARS-CoV-2-Antikörpern N2 - Übergeordnetes Ziel der Arbeit war die Entwicklung und Optimierung eines Suspensionsarray-Fluoreszenzimmunoassays (SAFIA) für die simultane Bestimmung verschiedener gegen SARS-CoV-2-Proteine gerichtete Antikörper mittels Multiplexdetektion in komplexen Matrices wie humanen Blutserumproben. KW - SARS-CoV-2 KW - Corona KW - COVID-19 KW - Coronavirus KW - Virus KW - Spike-Protein KW - Nucleocapsid-Protein KW - RBD KW - SAFIA KW - LFIA KW - ELISA KW - Partikel KW - Mutationen KW - Neutralisierende Antikörper KW - Durchflusszytometrie KW - ACE2 PY - 2022 SP - 1 EP - 99 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54722 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bienwald, Frank T1 - Optimierung der Aminosäureanalytik aromatischer Aminosäuren mittels HPLC N2 - Ausgehend von dem in der Literatur beschriebenen Verfahren zur Bestimmung aromatischer Aminosäuren konnte eine Analysemethode zur Proteinbestimmung über die optische Detektion von Tyrosin und Phenylalanin nach chromatographischer Trennung der Protein-Hydrolysate entwickelt werden, die gegenüber dem Verfahren aus der Literatur erhebliche Vorteile besitzt. Der Einsatz von Rundbodenvials stellt eine Neuerung und kostengünstige Alternative zu der konventionellen Hydrolyse in Vakuumhydrolyseröhrchen wie auch zu den Mikrowellenvials der Mikrowellenhydrolyse dar, die das Potential für Miniaturisierungen der Proben hat und sich zudem für große Probendurchsätze eignet. Anstelle der Mikrowellenheizungen wurde ein konventionelles Ölbad als Heizquelle verwendet. Somit ergibt sich eine Verbesserung auch darin, dass diese Methode geringere Geräteinvestitionen erfordert. Wie die Ergebnisse nahelegen, sind sowohl Salzsäure als auch Bromwasserstoffsäure geeignete Reagenzien, die bei der sauren Hydrolyse von Proteinen verwendet werden können. Mit Hilfe antioxidativer Zusätze können Nebenreaktionen erfolgreich vermieden werden. Hier haben sich L-Cystein und Oxalsäure als wirkungsvolle Additive herausgestellt. Wichtige Verbesserungen betreffen vor allem die Zeitersparnis bei der Hydrolyse, die Aufarbeitung der Hydrolysate und die chromatographischen Separationen. Erstere konnte gegenüber der konventionellen Methode von 22 Stunden auf 45 Minuten reduziert werden. Die chromatographische Trennung wurde so weit optimiert, dass die Laufzeit von 64 auf 35 Minuten verkürzt werden konnte. Zudem konnte auf das zeitraubende und kontaminationsanfällige Eindampfen der Hydrolysate verzichtet werden. Während der Aufarbeitung der Hydrolysate konnten die Menge eingesetzter Chemikalien reduziert und damit mögliche Störungen während der optischen Detektion verringert werden. Letztere wurde zum einen durch das Einbeziehen der UV-Absorption bei 260 nm erweitert, sodass eine Alternative zur Absorption bei 215 nm vorliegt, die ebenere Basislinien im Chromatogramm ermöglicht. Zum anderen wurde gezeigt, dass mit Hilfe der Fluoreszenz die Empfindlichkeit der Methode gegenüber der UV-Absorption erheblich verbessert werden kann. Anhand der Probe eines Birkenpollenextraktes ließ sich die Anwendbarkeit der optimierten Methode auf Realproben demonstrieren. KW - Aromatische Aminosäuren KW - Aromatic amino acid analysis KW - AAAA KW - Phenylalanine KW - Tyrosine KW - Hydrochloric acid KW - Hydrobromic acid KW - HCl KW - HBr KW - Chromatographie KW - Reversed-phase KW - Hydrolysis KW - AdvanceBio Peptide Map KW - PRP-C18 PY - 2017 SP - 1 EP - 71 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54650 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bahri, Marwa T1 - Ortsspezifische Biokonjugation von humanen Antikörpern mit IgG-bindenden Peptiden N2 - Es wurde im Rahmen dieser Arbeit eine neue Methode der Biokonjugation entwickelt, die es ermöglicht humane Antikörper ortspezifisch mit IgG-bindenden Peptiden zu konjugieren. Als Basis fungierte ein Peptid, welches für den Einsatz gezielt modifiziert wurde. So sollte am C-Terminus ein Biotin eingefügt werden, dass für die spätere Detektion der Biokonjugation genutzt werden kann, während am N-Terminus ein Cross-Linker für die kovalente Bindung zum Antikörper eingefügt wurde. Das Biotin wurde mittels Biotin-Lysin eingebaut. Dies hat den Vorteil, dass die modifizierte Aminosäure direkt in der SPPS genutzt werden kann. Auch der Cross-Linker soll schon während der SPPS in das Peptid integriert werden. Als Cross Linker wurden die zwei heterobifunktionellen Succinimidyl(3-bromoacetamid)propionate und Succinimidyl(4-iodacetyl)aminobenzoat untersucht. Die Aktivierung des Peptides mit dem SBAP-Cross-Linker erfolgte am besten im pH-Bereich zwischen 7,0 und 9,0. Die Modifizierung des Peptides mit dem Iodid-Cross-Linker SIAB unter den gleichen Bedingungen zeigte allerdings keine zufriedenstellenden Ergebnisse. Da das erste Peptid allerdings in den Folgeexperimenten sehr gute Ergebnisse zeigte, musste kein weiterer Linker getestet werden. Zusätzlich zu der Cross-Linker-Wahl sollte der Abstand zwischen dem Cross-Linker und dem Grundgerüst des Peptides auf den Einfluss der Bindung untersucht werden. Dazu wurden drei Kontrollpeptide synthetisiert, die entweder um zwei Aminosäuren zwischen dem ursprünglichen N-Terminus des Peptides und dem SBAP-Linker verlängert wurden, keinen SBAP-Linker beinhalten oder die Verlängerung ohne SBAP-Linker besaßen. Die erfolgreiche Synthese aller vier Peptide wurde mittels MALDI-TOF-MS bestätigt. KW - Peptide KW - Bioconjugation KW - Crosslinker PY - 2020 SP - 1 EP - 82 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54659 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Linke, Michael T1 - Entwicklung einer magnetischen Anreicherungsmethode für Peptidbibliotheken zur Identifizierung von Proteinbindern N2 - Das Ziel der Arbeit war die Entwicklung einer magnetischen Anreicherungsmethode für eine Bead-basierte Substanzbibliothek zur Identifizierung von Proteinbindern. Im Ramen des Forschungsbelegs wurde bereits eine Anreicherungsmethode für ein Modellsystem einer Peptidbibliothek entwickelt. Das Modellsystem bestand dabei aus zwei verschiedenen Peptiden. Als Positivkontrolle wurde das FLAG-Peptid gewählt, welches selektiv gegen den Anti-FLAG-Antikörper bindet, und ein weiteres Peptid wurde als Negativkontrolle gewählt. Anhand dieses Modellsystems konnte die zuvor entwickelte Anreicherungsmethode von 20.000 auf 1.000.000 Beads vergrößert werden. Hierbei wurde ein Anreicherungsfaktor von 818 und eine gute Wiederfindungsrate von 82% erreicht. KW - Peptide library KW - OBOC library KW - Enrichment KW - Magnetic beads KW - Protein interaction PY - 2018 SP - 1 EP - 86 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54651 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steglich, P. A1 - Rabus, D. G. A1 - Sada, C. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Mai, C. A1 - Mai, A. T1 - Silicon Photonic Micro-Ring Resonators for Chemical and Biological Sensing: A Tutorial N2 - Silicon photonic micro-ring resonators (MRR) developed on the silicon-on-insulator (SOI) platform, owing to their high sensitivity and small footprint, show great potential for many chemical and biological sensing applications such as label-free detection in environmental monitoring, biomedical engineering, and food analysis. In this tutorial,we provide the theoretical background and give design guidelines for SOI-based MRR as well as examples of surface functionalization procedures for label-free detection of molecules. After introducing the advantages and perspectives of MRR, fundamentals of MRR are described in detail, followed by an introduction to the fabrication methods, which are based on a complementary metal-oxide semiconductor (CMOS) technology. Optimization of MRR for chemical and biological sensing is provided, with special emphasis on the optimization of waveguide geometry. At this point, the difference between chemical bulk sensing and label-free surface sensing is explained, and definitions like waveguide sensitivity, ring sensitivity, overall sensitivity as well as the limit of detection (LoD) of MRR are introduced. Further, we show and explain chemical bulk sensing of sodium chloride (NaCl) in water and provide a recipe for label-free surface sensing. KW - Biosensors KW - Biophotonics KW - Chemosensor KW - Biosensor KW - Microresonator KW - Nanophotonics KW - Optical sensors KW - Photonic sensors KW - Optoelectronic KW - Ring resonator KW - Silicon photonics KW - Miniaturization KW - Lab-on-a-chip KW - Lab-on-chip KW - Waveguide KW - Surface chemistry KW - Silanization KW - Glutaraldehyde KW - Affinity immobilization KW - Antibody KW - Oriented immobilization KW - Real-time measurement PY - 2022 DO - https://doi.org/10.1109/JSEN.2021.3119547 SN - 1530-437X VL - 22 IS - 11 SP - 10089 EP - 10105 PB - IEEE AN - OPUS4-55147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Capabilities of using mobile platforms for monitoring hazard scenarios by the example of the RASEM project N2 - This presentation shows the capabilities of mobile platforms for monitoring hazard scenarios. As an example the RASEM project is presented. Furthermore two ideas for future work are shown, namely, Aerial-based Gas Tomography and Passive Smart Dust. T2 - Climate Change @ Fire Science Workshop CY - Berlin, Germany DA - 10.11.2022 KW - RASEM KW - Dust sensor KW - Low-cost KW - Sensor network KW - Passive Smart Dust KW - Gas Tomography PY - 2022 AN - OPUS4-56296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino A1 - Neumann, Patrick P. A1 - Weller, Michael G. T1 - Passive Smart Dust For Detection Of Hazardous Substances N2 - High demand for remote sensing of hazardous substances. Possible solution: Use of distributed, low cost, and environmentally safe particles as passive sensors that can be read out remotely Chemical intelligence on the particle surface can be easily modified Particles enable optically quantifiable response and inference of target substances (also no maintenance or power supply required T2 - 38th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Poros, Greece DA - 20.09.2022 KW - Smart Dust KW - Drone KW - Remote Detection KW - Colorchanging Particles PY - 2022 AN - OPUS4-56025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kaufmann, Jan Ole T1 - Finding the Ticking Timebomb - MRI probe for the detection of aneurysms N2 - Screening against ADAMTS4 reveals a specific peptide, which was turned into an MRI probe. The aneurysm in a mouse modal was visualized via MRI. A differentiation between stable and unstable aneurysm in an early state was performed. Using the probe as tool for an easy and non-invasive rupture assessment is possible. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - Magnetic resonance imaging KW - Peptide library KW - OBOC library KW - Synthetic peptides KW - Contrast agent KW - Imaging KW - ADAMTS4 KW - MALDI-TOF mass spectrometry KW - Cardiovascular diseases KW - Medicine KW - Diagnostic KW - Screening KW - Risk assessment KW - Aorta PY - 2022 AN - OPUS4-56313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, Gudrun A1 - Krahl, Thoralf A1 - Prinz, Carsten A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Luminescent properties of Eu3+/Tb3+ doped fluorine containing coordination polymers N2 - Lanthanides doped coordination polymers (CPs) with different binding motifs were synthesized to investigate the influence of the different fluorine positions in the structure on the decay time τ of the excited states. Fluorine can be integrated into the network mechanochemically via a fluorinated organic linker, here barium tetrafluoroterephthalate Ba(p-BDC-F4)2 or directly via a metal-fluorine bond (barium terephthalate fluoride BaF(p-BDC)0.5). The CP with a metal-fluorine bond shows the highest lifetime of the excited states of lanthanides (Eu3+, Tb3+ or Eu3+& Tb3+). The excitation of the lanthanides can be performed directly via the excitation wavelength typical for lanthanides and via the excitation wavelength of the linker. This enabled the simultaneous excitation of Eu3+ and Tb3+ in one CP. In the emission spectra (λem = 393 nm) of the mixed doped CPs (Eu3+ and Tb3+) the bands of both lanthanides can be observed. The integration into the crystal lattice and the homogeneous distribution of the lanthanides in the CPs is shown by X-ray diffraction, TEM, STEM-EDS measurements and the long decay times. KW - Alkaline earth metal coordination polymers KW - Fluorine coordination polymers KW - Lanthanides doped coordination polymers KW - Luminescence PY - 2021 DO - https://doi.org/10.1016/j.solidstatesciences.2021.106614 VL - 117 SP - 106614 PB - Elsevier Masson SAS AN - OPUS4-52559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska ED - de Oliveira Guilherme Buzanich, Ana ED - Strange, R. W. T1 - Time- and spatial-resolved XAFS spectroscopy in a single shot: new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ–2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 mm is achieved. KW - Single-shot XAFS KW - Time resolution PY - 2016 UR - http://scripts.iucr.org/cgi-bin/paper?S1600577516003969 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 VL - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Liverpool, UK AN - OPUS4-35903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Misra, Archismita T1 - Polyoxometalate Ionic Liquids (POM-ILs) as Protective Coatings for CulturalHeritage against Acid Corrosion and Biodeterioration N2 - Corrosion of stone by acid rain anddeterioration from microbial biofilmsare challenges pertinent worldwide forindustrial or residential buildings as wellas cultural heritage artefacts, like statuesor historic buildings. One mitigationoption might be the use of thintransparent films of polyoxometalate-based ionic liquids (POM-ILs). In thisregard, different limestone samples werecoated with hydrophobic, acid resistantPOM-ILs which also have biocidalproperties.1 Exposure of the samples tosimulated acid rain showed negligiblecorrosion compared to the significantdeterioration of unprotected samples(Fig 1. Left). In addition, the biocidalproperties of the POM-ILs suppress theformation of biofilms on coated stoneslabs. The coating is mechanically stableand is not removed even by harshmechanical and chemical treatment.Following studies successfully exploredthe effectiveness of the coating againstlampenflora growing in the PommeryChampagne cellar 2 (Fig 1. Right); andthe long-term performance of POM-ILsunder outdoor environmental conditions3. So, POM-ILs are already proven topossess remarkable anticorrosion andantimicrobial properties against aerobicmicroorganisms and being water-insoluble, they don’t get leached intoaquatic ecosystem, which is extremelybeneficial from an environmentalsustainability and toxicological point ofview. The current project aims tocontinue the journey on protecting thecultural heritage, shifting focus fromstones to metals and employ functionalPOM-IL nanocoatings to prevent MIC(Microbiologically Influenced Corrosion)of cultural heritage artefacts made ofmetal or metal alloy like carbon steel,brass, cast iron or bronze. Performanceof both the coating materials and coatingtechniques via optimization of theadhesion of the nanocoating on themetallic surface on the corrosion rateand corrosion products in the MICcaused by anaerobic microorganismslike methanogenic archaea or SulphateReducing Bacteria (SRB) would betested. The objective is to establishPOM-ILs as efficient environmentallysustainable nanocoating materialsagainst biocorrosion citing the already published success stories; and sketch theongoing endeavours and prospects ofthese very efficient candidates in thecontext of MIC mitigation. T2 - Mitigation of Microbiologically InfluencedCorrosion: Towards Scientific &Industrial Standardization (MIC-STAND) CY - Lisbon, Portugal DA - 24.07.2024 KW - Microbiologically influenced corrosion (MIC) KW - Polyoxometalate Ionic Liquid KW - Nanocoating KW - Cultural heritage PY - 2024 AN - OPUS4-64575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Misra, Archismita T1 - Polyoxometalate Ionic Liquids (POMILs) as Protective Coatings for Cultural Heritage Against Acid Corrosion and Biodeterioration N2 - Corrosion of stone by acid rain anddeterioration from microbial biofilms are challenges worldwide present forindustrial or residential buildings as wellas cultural heritage, like statues orhistoric buildings. One option is the useof thin transparent films ofpolyoxometalate-based ionic liquids(POM-ILs). Stone samples were coatedwith hydrophobic, acid resistant POM-ILs which also have biocidal properties.1Exposure of the samples to simulatedacid rain showed negligible corrosioncompared to the significant deteriorationof unprotected samples (Fig 1. Left). Inaddition, the biocidal properties of thePOM-ILs suppress the formation ofbiofilms on coated stone slabs. Thecoating is mechanically stable and is notremoved even by harsh mechanical andchemical treatment. Following studiessuccessfully explored the effectiveness ofthe coating against lampenflora growingin the Pommery Champagne cellar 2 (Fig1. Right); and the long-termperformance of POM-ILs under outdoorenvironmental conditions 3. So, POM-ILs are already proven to possessremarkable anticorrosion andantimicrobial properties against aerobicmicroorganisms and being water-insoluble, they don’t get leached intoaquatic ecosystem, which is extremelybeneficial from an environmentalsustainability and toxicological point ofview. The current project aims tocontinue the journey on protecting thecultural heritage, shifting focus fromstones to metals and employ functionalPOM-IL nanocoatings to prevent MIC(Microbiologically Influenced Corrosion)of cultural heritage artefacts made ofmetal or metal alloy like carbon steel,brass, cast iron or bronze. Performanceof both the coating materials and coatingtechniques via optimization of theadhesion of the nanocoating on themetallic surface on the corrosion rateand corrosion products in the MICcaused by anaerobic microorganismslike methanogenic archaea or SulphateReducing Bacteria (SRB) would betested. The objective would be toestablish POM-ILs as efficientenvironmentally sustainablenanocoating materials againstbiocorrosion citing the already publishedsuccess stories; and sketch the ongoingendeavours and prospects of these veryefficient candidates in the context ofbiocorrosion T2 - International Biodeterioration and Biodegradation Symposium CY - Berlin, Germany DA - 09.09.2024 KW - Microbiologically influenced corrosion (MIC) KW - Polyoxometalate Ionic Liquid KW - Nanocoating KW - Cultural heritage PY - 2024 AN - OPUS4-64576 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - Bhattacharya, Biswajit A1 - Rodríguez Sánchez, Noelia A1 - Gugin, Nikita T1 - Advancing sustainable synthesis through in situ monitoring and industrial scale-up of mechanochemical processes N2 - Mechanochemistry has emerged as a powerful approach for sustainable materials synthesis and processing, with significant potential to meet the UN Sustainable Development Goals. This presentation will highlight our recent advancements in understanding, monitoring, and scaling-up mechanochemical transformations, focusing on the balance between fundamental understanding of reaction mechanisms and its practical applications in energy storage and energy transfer materials. Our research has made significant strides in elucidating the fundamental mechanisms of mechanochemical reactions. We have investigated delayed polymorphism under mechanochemical conditions, revealing new insights into the interplay between mechanical impact, thermal effects, and structural transformations in molecular crystals. By employing variable temperature ball milling, we have demonstrated unprecedented control over polymorphic forms in organic cocrystals, opening new avenues for tailoring material properties. A central focus of our work has been the development and application of time-resolved in situ monitoring techniques for mechanochemical processes. Our research on real-time synchrotron X-ray diffraction has enabled unprecedented insights into reaction pathways and kinetics. Recently, we have successfully applied energy-dispersive X-ray diffraction for time-resolved in situ monitoring of reactive extrusion, marking a significant step towards ‘lighting up’ industrial-scale mechanochemistry. Bridging fundamental understanding with practical applications, we have explored the mechanochemical synthesis of functional materials for energy storage and transfer, making process in the mechanochemical synthesis of highly proton-conductive metal phosphonates, demonstrating the potential of mechanochemistry to manufacture advanced materials for energy applications. Addressing the challenges of industrial scale-up, we have investigated the role of solvent polarity in mechanochemical reactions, providing valuable guidance for optimizing organic syntheses such as the Knoevenagel condensation. This work contributes to our broader efforts to develop more efficient and sustainable chemical manufacturing processes. Looking to the future, we will discuss emerging directions in mechanochemistry, including the development of continuous flow processes and the integration of machine learning approaches for reaction prediction and optimization. As we anticipate the next decade of research, we envision mechanochemistry playing an increasingly crucial role in sustainable chemical manufacturing and materials processing, with far-reaching implications for addressing global energy and environmental challenges. T2 - Mech’cheM 2025: New forces in Mechanochemistry Conference CY - Montpellier, France DA - 04.06.2025 KW - Phosphonates KW - Biocomposites PY - 2025 AN - OPUS4-64845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - Bhattacharya, Biswajit A1 - Rodríguez Sánchez, Noelia A1 - Gugin, Nikita T1 - Mechanochemical innovations for sustainable synthesis of framework materials and industrial scaleup N2 - Mechanochemistry has emerged as a powerful approach for sustainable materials synthesis and processing, with significant potential to meet the UN Sustainable Development Goals. This presentation will highlight our recent advancements in understanding, monitoring, and scaling-up mechanochemical synthesis of framework materials, focusing on the balance between fundamental understanding of reaction mechanisms and its practical applications in energy storage and energy transfer materials. A central focus of our work has been the development and application of time-resolved in situ monitoring techniques for mechanochemical processes. Our research on real-time synchrotron X-ray diffraction has enabled unprecedented insights into reaction pathways and kinetics. Recently, we have successfully applied energy-dispersive X-ray diffraction for time-resolved in situ monitoring of reactive extrusion, marking a significant step towards ‘lighting up’ industrial-scale mechanochemistry. Bridging fundamental understanding with practical applications, we have explored the mechanochemical synthesis of functional materials for energy storage and transfer, making process in the mechanochemical synthesis of highly proton-conductive metal phosphonates, demonstrating the potential of mechanochemistry to manufacture advanced materials for energy applications. T2 - 17. international-conference für Materialchemie CY - Edinburgh, United Kingdom DA - 07.07.2025 KW - MOF KW - Synchrotron KW - ZIF PY - 2025 AN - OPUS4-64841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mazzeo, P A1 - Lampronti, G A1 - Michalchuk, Adam A1 - Belenguer, A A1 - Bacchi, A A1 - Emmerling, Franziska T1 - Accurate extrinsic and intrinsic peak broadening modelling for time-resolved in situ ball milling reactions via synchrotron powder X-ray diffraction N2 - The debate on the mechanisms which underpin mechanochemical reactions via ball mill grinding is still open. Our ability to accurately measure the microstructural (crystal size and microstrain) evolution of materials under milling conditions as well as their phase composition as a function of time is key to the in-depth understanding of the kinetics and driving forces of mechanochemical transformations. Furthermore, all ball milling reactions end with a steady state or milling equilibrium – represented by a specific phase composition and relative microstructure – that does not change as long as the milling conditions are maintained. The use of a standard sample is essential to determine the instrumental contribution to the X-ray powder diffraction (XRPD) peak broadening for time-resolved in situ (TRIS) monitoring of mechanochemical reactions under in operando conditions. Using TRIS-XRPD on a ball milling setup, coupled with low-energy synchrotron radiation, we investigated different data acquisition and analysis strategies on a silicon standard powder. The diffraction geometry and the microstructural evolution of the standard itself have been studied to model the instrumental contribution to XRPD peak broadening throughout the grinding activity. Previously proposed functions are here challenged and further developed. Importantly, we show that minor drifts of the jar position do not affect the instrumental resolution function significantly. We here report and discuss the results of such investigations and their application to TRIS-XRPD datasets of inorganic and organic ball mill grinding reactions. KW - Mechanochemistry KW - In situ diffraction KW - Synchrotron radiation KW - Sustainable chemisry PY - 2022 DO - https://doi.org/10.1039/d2fd00104g SP - 1 EP - 17 PB - Royal Society of Chemistry AN - OPUS4-55932 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lakshmipathi, M. A1 - Dey, S. A1 - Emmerling, Franziska A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam T1 - Designing Dual Mechanical Response in Molecular Crystals through Cocrystallization N2 - Two isomorphous crystals are reported based on a naphthylvinylpyridine coformer. The crystals are mechanically flexible and exhibit photosalient response to UV irradiation. We therefore show how multiple mechanical phenomena can be simultaneously designed into a single material by cocrystallization. KW - Cocrystal KW - Mechanical response PY - 2022 DO - https://doi.org/10.1021/acs.cgd.2c00913 SN - 1528-7483 VL - 22 SP - 6838 EP - 6843 PB - ACS Publ. CY - Washington, DC AN - OPUS4-56561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gnutzmann, Tanja A1 - Nguyen, Thi Yen A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Solvent-triggered crystallization of polymorphs studied in situ N2 - The crystallization of a highly polymorphic compound was studied in situ by combined time-resolved X-ray diffraction and Raman spectroscopy. Any influences of solid surfaces, temperature, and humidity on the crystallization were omitted by the use of a specially designed acoustic levitator. Investigations of polymorphic phase transitions during the crystallization process in different solvents allowed a structure assignment from first crystalline assemblies to final crystalline form. For the first time, it was possible to yield pure phases of selected polymorphs of the model compound ROY (5-methyl-2-[(2-nitrophenyl)amino]-3-thiophenecarbonitrile) directly from solution. The influence of the solvent on the final products and transient phases during the crystallization process was elucidated. KW - Polymorphism KW - Crystallization KW - In situ WAXS KW - In situ Raman spectroscopy KW - ROY PY - 2014 DO - https://doi.org/10.1021/cg501287v SN - 1528-7483 VL - 14 IS - 12 SP - 6445 EP - 6450 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-32583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Mechanochemical synthesis, characterization, and structure determination of new alkaline earth metal-tetrafluoroterephthalate frameworks: Ca(pBDC‑F4 )·4H2O, Sr(pBDC‑F4 )·4H2O, and Ba(pBDC‑F4 ) N2 - New fluorinated alkaline earth metal−organic frameworks were successfully synthesized by milling of metal hydroxides M(OH)2 with tetrafluoroterephthalic acid H2 pBDC-F4. Both calcium- and strontium-tetrafluoroterephthalates are tetrahydrated, while the barium tetrafluoroterephthalate is free of coordinating water molecules. The two isomorphic structures Ca(pBDC-F4)·4H2O and Sr(pBDC-F4)·4H2O were solved from the powder diffraction data by ab initio structure determination and subsequent Rietveld refinement. The products were thoroughly characterized by elemental analysis, thermal analysis, magicangle spinning NMR, Fourier transform infrared spectroscopy, scanning electron microscopy imaging, and Brunauer−Emmett−Teller measurements. Our findings suggest that the mechanochemical synthesis route is a promising approach for the preparation of new fluorinated alkaline earth metal−organic frameworks. KW - Mechanochemistry KW - MOFs KW - XRD PY - 2016 UR - http://pubs.acs.org/doi/abs/10.1021/acs.cgd.5b01457 DO - https://doi.org/10.1021/acs.cgd.5b01457 SN - 1528-7483 VL - 16/4 SP - 1923 EP - 1933 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-35940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bach, S. A1 - Panthöfer, M. A1 - Bienert, Ralf A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Role of water during crystallization of amorphous cobalt phosphate nanoparticles N2 - The transformation of amorphous precursors into crystalline solids and the associated mechanisms are still poorly understood. We illuminate the formation and reactivity of an amorphous cobalt phosphate hydrate precursor and the role of water for its crystallization process. Amorphous cobalt phosphate hydrate nanoparticles (ACP) with diameters of ∼20 nm were prepared in the absence of additives from aqueous solutions at low concentrations and with short reaction times. To avoid the kinetically controlled transformation of metastable ACP into crystalline Co₃(PO₄)₂ × 8H₂O (CPO) its separation must be fast. The crystallinity of ACP could be controlled through the temperature during precipitation. A second amorphous phase (HT-ACP) containing less water and anhydrous Co₃(PO₄)₂ was formed at higher temperature by the release of coordinating water. ACP contains approximately five molecules of structural water per formula unit as determined by thermal analysis (TGA) and quantitative IR spectroscopy. The Co²+ coordination in ACP is tetrahedral, as shown by XANES/EXAFS spectroscopy, but octahedral in crystalline CPO. ACP is stable in the absence of water even at 500 °C. In the wet state, the transformation of ACP to CPO is triggered by the diffusion and incorporation of water into the structure. Quantitative in situ IR analysis allowed monitoring the crystallization kinetics of ACP in the presence of water. KW - Fluorapatite-gelatin nanocomposites KW - Calcium-carbonate KW - Zinc phosphate KW - Crystal-growth KW - Nucleation KW - Polymorphism PY - 2016 DO - https://doi.org/10.1021/acs.cgd.6b00208 SN - 1528-7483 SN - 1528-7505 VL - 16 IS - 8 SP - 4232 EP - 4239 PB - ACS Publications AN - OPUS4-37616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ciornii, Dmitri A1 - Hodoroaba, Vasile-Dan A1 - Benismail, Nizar A1 - Altmann, Korinna T1 - Project 2: Interlaboratory Comparison on detection and quantitative assessment of microplastics by use of spectroscopic and thermo-analytical methods N2 - Validated and standardized methods in microplastic analysis are indispensable for robust monitoring and regulation. Alongside also reference materials are urgently needed. An interlaboratory comparison (ILC) offers a powerful tool to address both these challenges. The present study aimed to compare the precision and accuracy of various methods for the detection and quantification of microplastic in a water-soluble matrix. Additionally, it evaluated the suitability of the test materials (containing environmentally relevant plastic polymers) to serve as reference materials for the microplastic analysis. In this ILC several most used thermo-analytical and spectroscopic methods have been addressed: Pyrolysis-Gas Chromatography Mass Spectrometry (Py-GC/MS), Thermal Extraction-Desorption Gas Chromatography Mass Spectrometry (TED-GC/MS), micro-Fourier Transform Infrared Spectroscopy (µ-FTIR), and micro-Raman Spectroscopy and Laser Direct Infrared Spectroscopy (LDIR). Microplastic powders of polyethylene (PE) and polyethylene terephthalate (PET) were used to assess suitability of the test materials (microplastic tablets) for method validation and use in the ILCs. The participants were guided with a SOP how to dissolve the test samples and, depending on their selected method, either quantify the number of particles (by the spectroscopic methods) or determine the mass fraction of microplastic particles per sample (by the thermo-analytical methods). KW - ILC KW - Microplastic KW - FTIR KW - Raman KW - TED-GC/MS KW - Py-GC/MS PY - 2024 SP - 1 EP - 16 AN - OPUS4-60612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Zientek, Nicolai A1 - Rump, Doreen A1 - Fischer, Franziska A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Make and break - Facile synthesis of cocrystals and comprehensive dissolution studies N2 - Mechanochemistry is increasingly used as a ‘green alternative’ for synthesizing various materials including pharmaceutical cocrystals. Herein, we present the mechanochemical synthesis of three new cocrystals containing the API carbamazepine (cocrystals CBZ:Indometacin 1:1, CBZ:Benzamide 1:1, and CBZ:Nifedipine 1:1). The mechanochemical reaction was investigated in situ documenting a fast and complete reaction within one minute. Online NMR spectroscopy proved the direct influence of the dissolution behaviour of the coformers to the dissolution behaviour of the API carbamazepine. The dissolution behaviour of the organic cocrystals is compared to the behaviour of the pure drug indicating a general applicability of this approach for detailed cocrystal dissolution studies. KW - Cocrystals KW - Carbamazepine KW - Mechanochemistry KW - Powder diffraction KW - Online NMR spectroscopy PY - 2017 DO - https://doi.org/10.1016/j.molstruc.2016.11.063 SN - 0022-2860 SN - 1872-8014 VL - 1133 SP - 18 EP - 23 AN - OPUS4-38664 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Freshwater compartments: Screening method for polymer identification and mass contents of microplastic particles using TED-GC-MS N2 - The pathways of plastics, especially of microplastic (MP), in environmental compartments, particularly in aquatic systems, are not well understood. The critical point is the lack of fast, harmonised methods for sampling, sample preparation and sample analysis. These three analytical steps are dependent on one another and must be optimised. In recent years, we developed a method for representative sampling and fast detection of MP in aqueous systems. The sampling in different freshwater bodies is performed in the field with a fractionated filtration system using mesh sizes of 500, 100 and 50 µm. For water with an intermediate or high content of suspended particular matter a minimum of 1000 L has to be filtered. In the lab, mesh sizes of 10 and 5 µm are used for further filtration. Subsequently, the water filtrates of the different particle size classes are sterilised, dried, weighed and homogenised, if necessary. Conventional methods for MP analysis are infrared and raman spectroscopy, giving information on the shapes and numbers of individually identified MP particles. Our focus is on the determination of mass contents of various polymers potentially contained in environmental samples. For qualitative and quantitative MP detection TED-GC-MS is used, a two-step method based on gas chromatography-mass spectrometry (GC-MS) with previous thermal extraction. This method not only enables us to screen the samples for characteristic marker-molecules, thus identifying single polymers, but furthermore allows the calculation of mass contents of individual polymers. In the present work, different freshwater compartments were exemplarily studied to identify containing polymers and calculate their mass content in MP particles. T2 - MICRO2018 CY - Lanzarote, Spain DA - 19.11.2018 KW - Microplastic KW - TED-GC-MS KW - Mass contents PY - 2018 AN - OPUS4-46739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Braun, U. T1 - Monitoring von Mikroplastik N2 - Der Vortrag gibt einen Überblick was bei der Analyse von Mikroplastik zu beachten ist und beschreibt die Vor- und Nachteile der TED-GC/MS. T2 - Abschlusstreffen MikroPlaTas CY - Online meeting DA - 23.06.2021 KW - Mikroplastik KW - TED-GC/MS KW - Mikroplastik-Analytik PY - 2021 AN - OPUS4-52916 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Novel Trypsin-functionalized Corundum Particles for Improved Antibody Digestion N2 - Therapeutic monoclonal antibodies are the fastest-growing class of biological agents and the development of reliable analytical methods for their quantification is becoming increasingly important. Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) represents one of the leading technologies for antibody quantification. The serin protease trypsin has emerged as the gold standard enzyme for digesting intact protein into peptides for this approach. However, many protocols exist that often lead to different results. However, many protocols exist that often lead to different results depending on the digestion procedure. In particular, the type and amounts of detergents added during sample preparation for protein unfolding before digestion is known to create undesirable structure modifications of proteins (e.g. carbamylation) and significant bias in measurement results by inhibiting enzyme activity. The source and nature of the enzyme itself can also have an influence, whereby immobilized variants are increasingly being used to improve their stability, minimize self-digestion and enable a higher substrate-enzyme ratio. Here, we explored the potential of a novel thermostable trypsin and surface-functionalized corundum particles for enhanced antibody digestion. For this purpose, the inactive proenzym was recombinantly produced in inclusion bodies of E. coli and successfully folded back into functional conformation via multi-stage dialysis using a cysteine-cystine redox system. After cleavage of the propeptide and purification of active variants, enzyme activity was comparable to commercially available trypsin product. In addition, produced trypsin showed increased thermal stability under typical digestion conditions compared to reference product. In solution digestion experiments of antibody have revealed that the thermostable variant demonstrates enhanced digestive efficacy compared to the wild type. Furthermore, APTES-silanization followed by polymerization of corundum surface prevent nonspecific protein adsorption during the protein digestion procedure and the immobilized enzyme still showed substrate activity after covalent binding. Compared to wild-type and a non-immobilized enzyme, the surface-functionalized thermostable variant showed increased activity at temperatures above 80°C. Thus, this novel type of trypsin particles promises to not only improve antibody digestion at high temperatures, but also to prevent self-digestion and enable the separation of trypsin from target peptides in LC–MS analysis. T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 11.11.2024 KW - Antibody Quantification KW - Corundum KW - Enzyme Immobilization KW - LC-MS/MS PY - 2024 AN - OPUS4-61680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Herrmann, Stefan T1 - Charakterisierung zweier monoklonaler Antikörper zur Detektion von Sprengstoffen N2 - In 2019 over 30 000 people were killed or injured by explosions caused by explosives like TNT, PETN, HMX and RDX. Therefore, highly sensitive assays for the detection of TNT are needed. In this study we compared two commercially available TNT antibodies: A1.1.1 and EW75C with a highly optimized indirect competitive ELISA based on a BSA-TNA conjugate. As a result, a precision profile for both antibodies was determined with a LOD of 170 pmol L-1 for the clone A1.1.1 and a LOD of 3,2 nmol L-1 for the clone EW75C. The measurements showed that the clone A1.1.1 is a highly sensitive antibody for the detection of TNT while the clone EW75C does show medium performance at most. In the cross-reactivity characterization of both antibodies many substances, closely related to the structure of TNT were tested. Both antibodies showed strong cross reactivity with trinitroaniline and trinitrobenzene. For the clone A1.1.1, which is known to originate from immunization of mice with an TNP-glycine-KLH conjugate, this has to be expected. Interestingly the clone EW75C, which was not characterized yet, showed similar behavior. This suggests a TNA-conjugate as immunogen for the EW75C antibody as well. None of both antibodies showed cross-reactions to the high explosives PETN, HMX and RDX. Also, the cross-reactions of nitro musks with the antibodies were investigated. Despite their prohibition, nitro musks are still used in Asia especially and are particularly popular in India. The overall superior clone A1.1.1 showed a significant cross-reactivity to musk ambrette. For practical reasons the influence of musk ambrette on this assay when used in natural environment should be investigated. In further experiments, the highly sensitive TNT antibody A1.1.1 was digested with papain to obtain monovalent Fab-fragments. Due to its high stability against the digestion, a custom protocol for the IgG1 subclass of mice, to which the clone A1.1.1 belongs, was developed, resulting in a quantitative digestion of the intact antibody to Fab fragments. The success of the digestion was determined with MALDI-TOF-MS and SDS-PAGE. It was shown that this protocol worked for many different antibodies of IgG1 subclass as well. KW - TNT KW - Trinitrotoluol KW - Nitroaromaten KW - Nitromoschus KW - Duftstoffe KW - ELISA KW - Immunoassay KW - Antibody KW - Explosives KW - Klon A1.1.1 KW - Klon EW75C KW - Fab Fragment KW - Kreuzreaktion KW - Crossreactivity KW - Precision Profile KW - Präzisionsprofil KW - Affinity KW - Affinitätskonstante KW - IC50 PY - 2020 SP - 1 EP - 113 PB - Hochschule für Technik und Wirtschaft Berlin - htw CY - Berlin AN - OPUS4-54556 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Remmler, Dario A1 - Schwaar, Timm A1 - Pickhardt, M. A1 - Donth, C. A1 - Mandelkow, E. A1 - Weller, Michael G. A1 - Börner, H. T1 - On the way to precision formulation additives: 2D-screening to select solubilizers with tailored host and release capabilities N2 - A 2-dimensional high-throughput screening method is presented to select peptide sequences from large peptide libraries for precision formulation additives, having a high capacity to specifically host a drug of interest and provide tailored drug release properties. The identified sequences are conjugated with poly(ethylene glycol) (PEG) to obtain peptide-PEG conjugates that proved to be valuable as solubilizers for small organic molecule drugs to overcome limitations of poor water-solubility and low bio-availability. The 2D-screening method selects peptide sequences on both (i) high loading capacities and (ii) preferred drug-release capabilities as demonstrated on an experimental Tau-protein aggregation inhibitor/Tau- deaggregator with potentials for an anti-Alzheimer disease drug (BB17). To enable 2D-screening, a one-bead one-compound (OBOC) peptide library was immobilized on a glass slide, allocating individual beads to permanent positions. While the first screening step involved incubation of the supported OBOC library with BB17 to identify beads with high drug binding capacities by fluorescence scanner readouts, the second step reveals release properties of the high capacity binders by incubation with blood plasma protein model solutions. Efficiently peptides with high BB17 capacities and either keeper or medium or fast releaser properties can be identified by direct sequence readouts from the glass slide supported resin beads via matrix-assisted laser desorption/ionization time-of-flight tandem mass spectrometry. Four peptides are synthesized as peptide-PEG solubilizers representing strong, medium, weak releasers and non-binders. Loading capacities reached up to 1:3.4 (mol drug per mol carrier) and release kinetics (fast/medium/slow) are in agreement with the selection process as investigated by fluorescence anisotropy and fluorescence correlation spectroscopy. The ability of BB17/conjugate complexes to inhibit the aggregation of Tau4RDΔK (four repeat Tau ((M)Q244-E372 with deletion of K280), 129 residues) in N2a cells is studied by a Tau-pelleting assay showing the modulation of cellular Tau aggregation. Promising effects such as the reduction of 55% of total Tau load are observed for the strong releaser additive. Studies of in vitro Thioflavin S Tau-aggregation assays show half-maximal inhibitory activities (IC50 values) of BB17/conjugates in the low micro-molar range. KW - Block copolymer KW - Drug transporters KW - Peptide library screening KW - Formulation additives PY - 2018 DO - https://doi.org/10.1016/j.jconrel.2018.06.032 SN - 0168-3659 SN - 1873-4995 VL - 285 SP - 96 EP - 105 PB - Elsevier CY - Amsterdam AN - OPUS4-45483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Juds, Carmen T1 - Biocombinatorially selected peptide-polymer conjugates as polypropylene binders N2 - Peptide-polymer bioconjugates combine oligopeptides with synthetic polymer blocks and can be used for various applications in material sciences. In recent years, bioconjugates were applied as compatibilizers and coatings. Biocombinatorial approaches, such as phage display, have been shown to yield strong binding peptides, which exhibit excellent coating properties as peptide-PEO conjugates. Phage display represents a widely exploited strategy to select peptides or proteins that exhibit highly specific affinity to various substrates. Following a phage display experiment, DNA sequencing of binding phage clones is required in order to get the sequence information of the binding peptides. Traditionally, random clone picking followed by Sanger sequencing was applied. However, this method may not necessarily identify the strongest binding clones. Next-generation sequencing made sequencing of whole phage libraries possible, which highly improved the selection of strong binders. Here, we show that the biocombinatorial method of phage display combined with next generation DNA sequencing of whole phage libraries represents a powerful tool for an application in material chemistry. Phage display is used to find specific target binding peptides for polypropylene surfaces (PP). PP binders are of particular interest because thus far gluing or printing on PP is challenging due to its low surface energy. Scripts for sequence data analysis were developed and promising sequences were synthesized as peptide-PEO conjugates. Fluorescence based adsorption experiments on PP surfaces led to the identification of strong binding sequences and a better understanding of the peptide-surface interactions. T2 - 257th National Meeting of the American-Chemical-Society (ACS) CY - Orlando, FL, USA DA - 31.03.2019 KW - Peptides KW - Surfaces KW - Phage Display KW - Peptide Library KW - Screening KW - Glue KW - Paint KW - Polyethylene Glycol KW - PEG KW - Next Generation Sequencing PY - 2019 AN - OPUS4-48837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hiller, Lukas T1 - Herstellung und Charakterisierung eines rekombinanten Anti-Tetanus-Antikörpers aus verschiedenen Säugerzelllinien N2 - Antikörper sind in der medizinischen Welt nicht mehr wegzudenken. Ihr Einsatz-Repertoire als Therapeutika für die Behandlung diverser Krankheiten und Infektionen weitet sich von Jahr zu Jahr mehr aus. Dabei basiert ein Großteil der verwendeten Antikörper zu diesem Zeitpunkt auf monoklonalen Antikörpern auf Basis von Hybridomazellen. Doch hier könnten rekombinante Antikörper aufgrund ihrer Vektor-basierten Expression eine vielversprechende und womöglich sogar revolutionierende Alternative bieten. So ergeben sich neue Optimierungsoptionen für Merkmale wie Affinität, Stabilität und Kompatibilität über Anpassungen auf genetischer oder posttranslationaler Ebene. Allerdings ergibt sich kein Anwendungszweck ohne die vorhergehende detaillierte Charakterisierung der Antikörper. Denn nur mit spezifischem Wissen über die diversen Eigenschaften und Wechselwirkungen kann eine effektive und präzise Verwendung in der Diagnostik und Therapeutik gewährleistet werden und auf diese Weise Leben retten. Aus diesem Grund beschäftigt sich diese Masterarbeit mit der Vertiefung der rekombinanten Antikörper-Thematik. Dazu soll ein Anti-Tetanus-Antikörper erstmals rekombinant in verschiedenen Zelllinien hergestellt und anschließend über umfangreiche analytische Verfahren mit einem Fokus auf die Einflussanalyse der unterschiedlichen posttranslationalen Glykosylierungen charakterisiert werden. Zu diesem Zweck wurden als Grundlage einerseits zwei P1316-Dual-Expressions-Vektoren mit variierenden Insert-Positionen der schweren und leichten Kette durch Gibson-Assembly sowie individuellen pRK5-Plasmide für eine separiert Expression der Antikkörperketten mithilfe Restriktionsfragment-Ligation generiert. In einer Gegenüberstellung der der Expressionsausbeuten stellte sich die Überlegenheit der P1316-Plasmid-Konfiguration heraus, in der das Leichtketten-Insert an der ersten Expressionsstelle positioniert ist. Deshalb wurde dieser Vektor als Ausgangspunkt für die anschließende hochskalierten Herstellung des Anti-Tetanus-Antikörpers in Expi293F-GnTI- und ExpiCHO-S-Zellen verwendet. Ein ELISA bestätigte die Bindungsaktivität der rekombinanten Antikörper am Tetanus-Toxoid unabhängig vom Expressionssystem. Nach einer folgenden Optimierung der für die Aufreinigung verwendeten Protein-A-Affinitätschromatographie, wurde über weitere Charakterisierungsmethoden wie Größenausschlusschromatographie und dynamische Lichtstreuung eine vergleichbare Aggregation aufgrund der sauren Elution aufgezeigt. In diesem Kontext wurde die Notwendigkeit einer Zweistufen-Präparation mit Affinitäts- und Größenausschlusschromatografie für den Erhalt monodisperser Proben verdeutlicht. Zudem wurden die verschiedenen intakten Massen mitsamt ihrer spezifischen Glykan-abhängigen Streumaßen in Relation zum monoklonalen NISTmAB-Referenzantikörper bestimmt. Dabei konnte den Erwartungen nach sowohl die geringere Masse als auch die uniformere Glykosylierung der in Expi293 GnTI- exprimierten Immunoglobuline in Relation zum ExpiCHO-S-Antikörper nachgewiesen werden. Anschließend wurde das Stabilitätsverhalten mittels thermischer Entfaltung und dynamischer Lichtstreuung über einen ausgeweiteten Zeitraum sowie verschiedenen Temperaturen dokumentiert. Grundlegend wurde eine höhere thermische Stabilität der zweiten konstanten Schwerketten-Domäne des aus ExpiCHO-S-Zellen stammenden Antikörpers nachgewiesen. Außerdem konnte eine problemlose Lagerungsfähigkeit beider unterschiedlich glykosylierter Antikörper bei Raumtemperatur für mindestens 4 Wochen festgestellt werden. Des Weiteren wurde die Langzeitlagerung im Rahmen der Auswirkung von Gefrier-Auftau-Zyklen mit gleichbleibenden Methoden sowie zusätzlicher Größenausschlusschromatographie erprobt. Hierbei stellte sich der Erhalt der strukturellen Integrität nach bis zu 15 Zyklen heraus. Allerdings geht die Monodispersität bereits nach wenigen Zyklen verloren, wobei die geringfügiger glykosylierten Expi293F-GnTI-Anti-Tetanus-Antikörper eine stärkere Beeinträchtigung durch multiple Gefrier-Auftau-Zyklen aufwiesen. KW - Rekombinante Antikörper KW - Affinitätschromatographie KW - Größenausschlusschromatographie KW - MALDI-TOF-MS KW - Dynamische Lichtstreuung PY - 2024 SP - 1 EP - 120 CY - Berlin AN - OPUS4-59865 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbas, Ioana M. A1 - Hoffmann, Holger A1 - Montes-Bayón, M. A1 - Weller, Michael G. T1 - Improved LC-MS/MS method for the quantification of hepcidin-25 in clinical samples N2 - Mass spectrometry-based methods play a crucial role in the quantification of the main iron metabolism regulator hepcidin by singling out the bioactive 25-residue peptide from the other naturally occurring N-truncated isoforms (hepcidin-20, -22, -24), which seem to be inactive in iron homeostasis. However, several difficulties arise in the MS analysis of hepcidin due to the sticky character of the peptide and the lack of suitable standards. Here, we propose the use of amino- and fluoro-silanized autosampler vials to reduce hepcidin interaction to laboratory glassware surfaces after testing several types of vials for the preparation of stock solutions and serum samples for isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). Furthermore, we have investigated two sample preparation strategies and two chromatographic separation conditions with the aim of developing an LC-MS/MS method for the sensitive and reliable quantification of hepcidin-25 in serum samples. A chromatographic separation based on usual acidic mobile phases was compared with a novel approach involving the separation of hepcidin-25 with solvents at high pH containing 0.1% of ammonia. Both methods were applied to clinical samples in an intra-laboratory comparison of two LC-MS/MS methods using the same hepcidin-25 calibrators with good correlation of the results. Finally, we recommend an LC-MS/MS-based quantification method with a dynamic range of 0.5–40 μg/L for the assessment of hepcidin-25 in human serum that uses TFA-based mobile phases and silanized glass vials. KW - HPLC KW - Liquid chromatography KW - Mass spectrometry KW - Silanization KW - Mobile phase KW - Adsorption KW - Peptide losses KW - Recovery KW - Validation KW - Quality control KW - QC KW - Iron disorders KW - Chronic kidney disease KW - Metrology KW - Round robin exercise KW - Basic solvent KW - Peptide analysis PY - 2018 DO - https://doi.org/10.1007/s00216-018-1056-0 SN - 1618-2642 SN - 1618-2650 VL - 410 IS - 16 SP - 3835 EP - 3846 PB - Springer Nature CY - Heidelberg AN - OPUS4-45053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Celasun, S. A1 - Remmler, D. A1 - Schwaar, Timm A1 - Weller, Michael G. A1 - Du Prez, F. A1 - Börner, H. G. T1 - Digging into the sequential space of thiolactone precision polymers: A combinatorial strategy to identify functional domains N2 - Functional sequences of precision polymers based on thiolactone/Michael chemistry are identified from a large one-bead one-compound library. Single-bead readout by MALDI-TOF MS/MS identifies sequences that host m-THPC that is a second Generation photo-sensitizer drug. The corresponding Tla/Michael-PEG conjugates make m-THPC available in solution and drug payload as well as drug release kinetics can be fine-tuned by the precision segment. KW - Combinatorial chemistry KW - Combinatorial polymer libraries KW - Sequence-defined oligomer KW - Precision polymer sequencing KW - Pseudo peptides KW - MALDI-TOF KW - ESI MS KW - Mass spectrometry KW - Sequencing KW - PEG KW - Polyethylene glycol KW - Solubilizer KW - Drug KW - Conjugates PY - 2019 DO - https://doi.org/10.1002/anie.201810393 SN - 1521-3773 VL - 58 IS - 7 SP - 1960 EP - 1964 PB - Wiley-VCH CY - Weinheim AN - OPUS4-47323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vranic, Marija T1 - Expression, purification and characterization of the recombinant cysteine-rich biomarker Hepcidin-25 N2 - Hepcidin regulates iron homeostasis in response to inflammation, erythropoietic demand, and iron stores. The native state of hepcidin-25 is an attractive target for the development of a reliable analytical tool that can quantify the hepcidin concentration in biological samples and reveal iron metabolic disorders. Therefore, a selective immunoassay would have to discriminate between different types of hepcidin and quantify only hepcidin-25’s concentration. The peptide contains a well-defined β-sheets and a β-hairpin loop stabilized by four disulfide bonds. Recently, it was shown that hepcidin-25 contains an ATCUN motif at its N-terminus. This motif is known to have high affinity towards Cu2+ and Ni2+. One of the aims of this study is to determine the three-dimensional (3D) structure of metal-bound hepcidin-25. Here, we present an optimized procedure for preparing natively folded hepcidin 25 (~2.80 kDa) and structural analysis of metal binding to hepcidin-25. Hepcidin was expressed as a His6-SUMO-hepcidin-25 fusion protein (~16.20 kDa) in Escherichia coli, Origami B strains, and purified as a soluble recombinant protein in three steps. After purification based on the nickel affinity chromatography, the purified His6-SUMO-hepcidin 25 fusion protein was cleaved by the SUMO-specific ULP1 protease. The liberated hepcidin 25 was further purified on a Superdex 30 16/600 column and folded in the last step of purification in the presence of glutathione. Freshly expressed hepcidin was kept in its reduced form to prevent misfolding and allow for efficient removal of the SUMO tag. The presence of natively folded hepcidin 25 after RP-HPLC was confirmed by ESI-MS and NMR spectroscopy. Based on published chemical shifts, we achieved a nearly complete assignment of the labeled and unlabeled hepcidin-25 at pH=3. Comparison of 1H chemical shifts and TOCSY spectra at pH=7 in the presence and absence of Ni2+ demonstrates that the metal binds at the N-terminus of hepcidin 25. Chemical shift changes due to metal complexation decrease further away from the metal binding site. T2 - 28th International Conference on Magnetic Resonance in Biological Systems, ICMRBS CY - Dublin, Irland DA - 19.08.2018 KW - Peptides KW - Metalloproteins KW - Copper KW - ATCUN KW - Nickel KW - NMR KW - SUMO KW - Fusion protein KW - Iron disorders KW - ESI-MS KW - RP-HPLC PY - 2018 AN - OPUS4-46944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Airborne Laser-Induced Plasma as an Ambient Desorption/Ionization Source for Mass Spectrometry and its Characterization N2 - Laser-induced plasma (LIP) has drawn significant amount of attentions in the past decades, particular in elemental analyses for solid or liquid samples. Through proper focusing of the highly energetic laser beam, the plasma can also be ignited in the ambient air, where airborne analytes can be ionized. Such an effect enabled the use of airborne LIP as an ambient ionization source for mass spectrometric analyses. In contrast to other ambient desorption/ionization sources, airborne LIP does not require a specific discharge medium or expensive gas stream. Meanwhile, the airborne LIP produces reagent ion species for both proton-transfer and charge-transfer reactions in addition to the vacuum ultraviolent photons that are capable of promoting single photon ionization, which can be utilized to ionize polar and non-polar analytes. In order to gauge the analytical performance of airborne LIP, it is critical to understand the undergoing chemistry and physics during and after the plasma formation. Due to the ambient nature of airborne LIP, the variations of air composition and flow strongly affect the plasma behaviors. Preliminary result suggested the addition of a laminar flow of nitrogen gas favored the formation of protonated species (MH+) against the molecular ones (M+). Although the gas addition approach cannot fully tune the ionization process towards the specific production of pseudo-molecular species versus molecular ones, the alternation of molecular ion formation can be used for analyte recognitions through post processing of the ion patterns. The pulsed character of the used lasers makes the reagent ion equilibrium both transient- and highly fluid-dynamically controlled. The acoustic shock-waves induced by the airborne LIP get affected by an applied gas streams towards the plasma center, influencing the molecular-ion and ion-ion interactions in the near proximity of the plasma. To understand the airborne LIP formation, the temporally and spatially resolved optical emission spectra were recorded. The results will be correlated to time-resolved mass-spectrometric investigations of the ion profile during different stages of the plasma formation. As one example, the formation of pyrylium ion originating from aromatic compounds will be highlighted. T2 - SciX 2018 CY - Atlanta, GA, USA DA - 21.10.2018 KW - Laser-Induced Plasma KW - Ambient Desorption/Ionization KW - Mass Spectrometry KW - Characterization PY - 2018 AN - OPUS4-46376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Costa, Elena T1 - Development of a rapid test for on-site measurement of pyrethroid surface residues N2 - Type-I pyrethroids are frequently used for disinfection purposes against insects such as adult mosquitoes, or diseases carried by insects, like Malaria or Zika in cabins of airplanes on long-distance flights especially from tropical destinations. This treatment is mandatory at various airports but compliance with the rules is difficult to test for. Moreover, if improperly used, these compounds can entail negative health effects for crews and passengers. The detection of the pyrethroids will be achieved thanks to an antibody-gated indicator delivery system (gAID) utilizing monoclonal antibodies and hybrid sensory nanoparticles. After the interaction of the pyrethroid with the gAID, the liberated indicator (dye) will be detected. Since only few analyte molecules are necessary for pore opening yet release a large number of dyes, the system shows intrinsic signal amplification. The device system to be developed has to be so simple that chemically untrained personnel, such as ground or cabin crew, can use it and obtain a result in a reasonably short period of time, e.g., ≤5 min. The need for high accuracy and sufficient sensitivity, established at 0.001 g m–2, is a critical requirement and imposes another significant challenge since this value is beyond current LFTs reported in the literature for pesticide detection to date. In order to achieve the selectivity and sensitivity required by the test itself, and to avoid cross reactivity with other type I pyrethroids, the production of a monoclonal antibody for both Permethrin and Phenontrin is necessary. The synthesis of the two hapten molecules and the subsequent immunization with different immunogens represent the first goal of the work. T2 - Rapid Methods Europe 2018 CY - Amsterdam, The Netherlands DA - 05.11.2018 KW - Pyrethroids KW - Raid test KW - Test strip KW - Delivery system KW - Air traffic PY - 2018 AN - OPUS4-47128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vranic, Marija T1 - Metal-binding properties of the cystein-rich biomarker Hepcidin-25 N2 - Hepcidin-25 regulates iron homeostasis in response to inflammation, erythropoietic demand and iron stores. The liver synthesizes three types of hepcidin, only hepcidin-25 indirectly regulates and coordinates use and storage of iron. Hepcidin-25 contains a well defined β-sheet and β-hairpin loop stabilized by four disulfide bonds. The N-terminus which plays a crucial role in the biological activity of hepcidin-25 was found to be disordered. The ATCUN motif sequence is present at the N-terminus (Asp-Thr-His). The ATCUN motif (H2N-X-X-His) binds Cu2+ and Ni2+ with high affinity and always contains histidine in its sequence. NMR provides an ideal tool to determine hepcidin-25’s threedimensional(3D) structure taking into account the Cu2+ and Ni2+ binding capacity of hepcidin’s ATCUN motif. T2 - 3rd International Conference Proteins and Peptides, Structure, Function and Biotechnology CY - Geneva, Switzerland DA - 23.07.2018 KW - Peptides KW - Metalloproteins KW - Chromatography KW - ATCUN KW - Nickel KW - Copper KW - SUMO KW - Fusion protein KW - Iron disorders KW - ESI-MS KW - RP-HPLC PY - 2018 AN - OPUS4-46945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vranic, Marija T1 - Metal-binding properties of the cysteine-rich biomarker Hepcidin-25 N2 - Comparison of 1H chemical shifts and TOCSY data in the presence and absence of Ni2+ demonstrates that the metal binds at the N-terminus of the hepcidin-25. Chemical shift changes due to metal complexation decrease further away from the metal binding site, with the smallest effect at phenylalanine [Phe-4], proline [Pro-5] and isoleucine [Ile-6]. T2 - 8th Peptide Engineering Meeting CY - Berlin, Germany DA - 08.11.2018 KW - Peptides KW - Metalloproteins KW - Copper KW - ATCUN PY - 2018 AN - OPUS4-46946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Martin T1 - Development of a biosensor for the online detection of explosives N2 - An affinity column, which removed up to 99 % of high affinity Anti-TNT antibody at high antibody concentrations, was manufactured based on a monolithic glass core and a trinitroaniline-BSA conjugate. To detect the label Dy654 in the nM range an epi-fluorescence microscope setup with a CMOS camera was established to serve as online fluorescence detector with multiplexing capabilities. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Online fluorescence KW - Trinitro KW - Affinty KW - Antibody PY - 2019 AN - OPUS4-47745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino A1 - Neumann, Patrick P. A1 - Weller, Michael G. T1 - Drone-based Localization of Hazardous Chemicals by Passive Smart Dust N2 - We introduce a passive smart dust concept as a novel solution for environmental monitoring. Utilizing chemical reagents like colorimetric indicators and other chemosensors, these particles detect varying environmental conditions. We developed paper-based sensors that are both cost-effective and eco-friendly. In practical tests, these sensors, dispersed over a designated area, successfully identified hazardous substances by changing their color when exposed to acids or bases. This color change was remotely detectable using a drone-mounted color camera. The data thus obtained was processed through specialized software, accurately pinpointing areas of contamination. This method proves the efficacy and scalability of passive smart dust technology for real-time, environmentally sustainable remote sensing of hazardous materials T2 - 2024 IEEE International Symposium on Olfaction and Electronic Nose (ISOEN) CY - Grapevine, Texas, USA DA - 12.05.2024 KW - Indicator KW - Passive Smart Dust KW - Colorimetric Sensor KW - Drone KW - Cellulose KW - Environmental Monitoring KW - Confetti KW - Hazard Detection PY - 2024 SN - 979-8-3503-7053-9 VL - 1 SP - 1 EP - 3 PB - IEEE CY - Piscataway, NJ 08855-1331 USA AN - OPUS4-60176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino A1 - Neumann, Patrick P. A1 - Weller, Michael G. T1 - Passive Smart Dust a versatile low-cost sensor platform N2 - Coated cellulose particles as colourimetric passive sensors that are detected by the optical camera system of a drone. In this way, hazardous substances, e.g. acids, can be detected from a safe distance in a cost-effective and environmentally friendly way. N2 - Beschichtete Zellulose Partikel als kolorimetrische passive Sensoren, die mittels optische Kamerasystem einer Drohne erfasst werden. Somit können Gefahrenstoffe, in ersten Versuchen zB Säuren aus sicherer Entfernung, kostengünstig und umweltverträglich detektiert werden. T2 - SMSI 2023 Sensor and Measurement Science International CY - Nuremberg, Germany DA - 08.05.2023 KW - Passive Smart Dust KW - Drone KW - Colorimetric sensor particles KW - Remote detection PY - 2023 DO - https://doi.org/10.5162/SMSI2023/C5.3 SP - 1 EP - 2 AN - OPUS4-57527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino T1 - Passive Smart Dust: A versatile low-cost sensor platform N2 - Beschichtete Zellulose Partikel als kolorimetrische passive Sensoren, die mittels optische Kamerasystem einer Drohne erfasst werden. Somit können Gefahrenstoffe, in ersten Versuchen z. B. Säuren aus sicherer Entfernung, kostengünstig und umweltverträglich detektiert werden. T2 - SMSI 2023 Sensor and Measurement Science International CY - Nuremberg, Germany DA - 08.05.2023 KW - Passive Smart Dust KW - Drone KW - Colorimetric sensor particles PY - 2023 AN - OPUS4-57526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mangarova, Dilyana Branimirova T1 - A novel ADAMTS-specific MR peptide probe for characterization of atherosclerotic plaques in a murine model N2 - Motivation: A precise diagnosis of atherosclerosis is of clinical importance, since cardiovascular disease remain one of the leading causes of death worldwide. Goal(s): The goal of this study was to evaluate the feasibility of characterizing a disintegrin and metalloproteinase with thrombospondin motifs (ADAMTS4) using molecular magnetic resonance imaging in a preclnical model of atherosclerosis. Approach: Molecular magnetic resonance imaging using a novel probe targeted against ADAMTS4 was used in a high-fat murine model. Results: It was possible to image atherosclerotic lesions in a mouse model using an ADAMTS4- specific probe for magnetic resonance imaging. Impact: Using molecular MRI targeting ADAMTS4 is a promising method for characterization of plaque composition and could possibly impact plaque vulnerability assessment in the diagnosis and treatment of atherosclerosis in patients. N2 - Motivation: Eine genaue Diagnose der Atherosklerose ist von klinischer Bedeutung, da Herz-Kreislauf-Erkrankungen nach wie vor eine der häufigsten Todesursachen weltweit sind. Ziel(e): Ziel dieser Studie war es, die Durchführbarkeit der Charakterisierung einer Desintegrin- und Metalloproteinase mit Thrombospondin-Motiven (ADAMTS4) mittels molekularer Magnetresonanztomographie in einem präklinischen Modell der Atherosklerose zu untersuchen. Herangehensweise: Molekulare Magnetresonanztomographie mit einer neuartigen, gegen ADAMTS4 gerichteten Sonde wurde in einem fettreichen Mausmodell eingesetzt. Ergebnisse: Es war möglich, atherosklerotische Läsionen in einem Mausmodell mit einer ADAMTS4-spezifischen Sonde für die Magnetresonanztomographie abzubilden. Auswirkungen: Die Verwendung einer molekularen MRT, die auf ADAMTS4 abzielt, ist eine vielversprechende Methode zur Charakterisierung der Plaque-Zusammensetzung und könnte sich möglicherweise auf die Bewertung der Plaque-Anfälligkeit bei der Diagnose und Behandlung von Atherosklerose bei Patienten auswirken. T2 - 2024 ISMRM & ISMRT Annual Meeting & Exhibition CY - Singapore DA - 04.05.2024 KW - ADAMTS4 KW - Peptide probe KW - Peptide binder KW - Selective peptide KW - International Society for Magnetic Resonance in Medicine PY - 2024 AN - OPUS4-60865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hernández García, María Amparo T1 - SAF-based optical biosensor with 3D-printed free-form optics for targeted explosives immuno-detection N2 - Guaranteeing safety and security of citizens requires a significant effort and innovative tools from national and international agencies and governments, especially when it comes to the field of explosives detection. The need to detect Improvised Explosive Devices (IEDs) and Home-made Explosives (HMEs) at a point of suspicion, has grown rapidly due to the ease with which the precursors can be obtained and the reagents synthesised. The limited availability of immunoanalytical tools for HME detection presents an opportunity for the development of new devices, which enable a rapid detection and recognise the target analyte with high specificity and sensitivity. In this work, we introduce an optical biosensor for highly specific and sensitive HME detection. The immunoassay system is placed in a hydrogel environment permeable to the analyte and transparent to light interrogating the fluorescently labelled antibodies. The readout of the immunoanalytical system is realized with Supercritical Angle Fluorescence (SAF), an advanced microscopy technique. To accomplish this, we made use of recent, commercial high resolution (< 22 µm) Liquid Crystal Display 3D printers to fabricate a parabolic optical element with high refractive index (RI>1.5) and transmission values (>90%) from photo-resin. Aiming at a new generation of sensors, which not only can meet the requirements of trace detection, but can also be used for substance identification, the combination of immunoanalytical recognition with SAF detection offers a modularity and versatility that is principally well suitable for the measurements of target analytes at trace levels. T2 - 8th International conference in Biosensing Technology CY - Seville, Spain DA - 12.05.2024 KW - 3D printing KW - Biosensor KW - Fluorescence KW - Explosives PY - 2024 AN - OPUS4-60561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -