Chemische Charakterisierung und Spurenanalytik
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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (158)
- 1.1 Anorganische Spurenanalytik (46)
- 6 Materialchemie (40)
- 1.4 Prozessanalytik (38)
- 1.6 Anorganische Referenzmaterialien (28)
- 1.7 Organische Spuren- und Lebensmittelanalytik (28)
- 1.8 Umweltanalytik (28)
- 6.6 Physik und chemische Analytik der Polymere (21)
- 6.3 Strukturanalytik (18)
- 1.9 Chemische und optische Sensorik (13)
Eingeladener Vortrag
- nein (98)
The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for health, food and environmental matters. Monensin (MON) is an ionophore antibiotic widely used to cure and prevent coccidiosis by chicken especially in broiler farming. Residues can be found in food products (chicken and eggs) and in the environment (manure, soil, water). Several transformation processes can alter the parent compound MON, ranging from biotransformation in living organism to biotic/abiotic and microbial processes in environmental matters.
The main objective of this work was to investigate the potential of electrochemistry (EC) to simulate oxidative transformation processes of MON and to predict TPs. An electrochemical reactor was used consisting of a flow-through cell with a glassy carbon working electrode. Derived TPs were analyzed by online coupling of EC and high-resolution mass spectrometry (HRMS) and LC/HRMS offline measurements. Among the generated TPs already known as well as unknown TPs of MON could be found.
Additionally, MON was subjected also to other transformation experiments like metabolism tests with rat microsomes or the pH-dependent hydrolysis. As a result, different targeted and suspected TPs could be identified by analysis with LC/HRMS.
An overview of detected/identified TPs from this study will be presented in comparison to literature known metabolites and TPs.
Rationale: Boron (B) is an essential micronutrient in plants and its isotope variations are used to gain insights into plant metabolism, which is important for crop plant cultivation. B isotope variations were used to trace intra‐plant fractionation mechanisms in response to the B concentration in the irrigation water spanning the
range from B depletion to toxic levels.
Methods: A fully validated analytical procedure based on multi‐collector inductively coupled plasma mass spectrometry (MC‐ICP‐MS), sample decomposition and B Matrix separation was applied to study B isotope fractionation. The Validation was accomplished by establishing a complete uncertainty budget and by applying reference materials, yielding expanded measurement uncertainties of 0.8‰ for pure boric acid solutions and ≤1.5‰ for processed samples. With this validated procedure SI traceable B isotope amount ratios were determined in plant reference materials for the first time.
Results: The B isotope compositions of Irrigation water and bell pepper samples suggest passive diffusion of the heavy 11B isotope into the roots during low to high B concentrations while uptake of the light 10B isotope was promoted during B depletion, probably by active processes. A systematic enrichment of the heavy 11B isotope in higher located plant parts was observed (average Δ11Bleaf‐roots = 20.3 ± 2.8‰ (1 SD)), possibly by a facilitated transport of the heavy 11B isotope to growing Meristems by B transporters.
Conclusions: The B isotopes can be used to identify plant metabolism in Response to the B concentration in the irrigation water and during intra‐plant B transfer. The large B isotope fractionation within the plants demonstrates the importance of
biological B cycling for the global B cycle.
19th and 20th centuries glass paint layers consist of a colour body and a colourless lead silicate flux, in which borax or boric acid was added as further component to improve the paint ability and to reduce the firing temperature for multiple layers of paint. Model glasses were used in laboratory tests to investigate the stability of glass paints with additions of boron oxide. To determine boron in paint layers, a LIBS-system with pulsed NdYAG-laser was used.
Tempeh is a common food in Indonesia, produced by fungal fermentation of soybeans using Rhizopus sp., as well as Aspergillus oryzae, for inoculation. Analogously, for economic reasons, mixtures of maize and soybeans are used for the production of so-called tempeh-like products. For maize, a contamination with the mycoestrogen zearalenone (ZEN) has been frequently reported. ZEN is a mycotoxin which is known to be metabolized by Rhizopus and Aspergillus species. Consequently, this study focused on the ZEN transformation during tempeh fermentation. Five fungal strains of the genera Rhizopus and Aspergillus, isolated from fresh Indonesian tempeh and authentic Indonesian inocula, were utilized for tempeh manufacturing from a maize/soybean mixture (30:70) at laboratory-scale. Furthermore, comparable tempeh-like products obtained from Indonesian markets were analyzed. Results from the HPLC-MS/MS analyses show that ZEN is intensely transformed into its metabolites alpha-zearalenol (alpha-ZEL), ZEN-14-sulfate, alpha-ZEL-sulfate, ZEN-14-glucoside, and ZEN-16-glucoside in tempeh production. alpha-ZEL, being significantly more toxic than ZEN, was the main metabolite in most of the Rhizopus incubations, while in Aspergillus oryzae fermentations ZEN-14-sulfate was predominantly formed. Additionally, two of the 14 authentic samples were contaminated with ZEN, alpha-ZEL and ZEN-14-sulfate, and in two further samples, ZEN and alpha-ZEL, were determined. Consequently, tempeh fermentation of ZEN-contaminated maize/soybean mixture may lead to toxification of the food item by formation of the reductive ZEN metabolite, alpha-ZEL, under model as well as authentic conditions.
Der Vortrag beschreibt den Entwicklungsprozess des Analysenverfahrens TED-GC-MS zur Bestimmung von Mikroplastikgehalten in Umweltproben im Rahmen des BMBF-Projektes MiWa. Die Funktionsweise, die Automatisierung und die Optimierung einzelner Geräteparameter und Leistungsdaten werden gezeigt. Untersuchungen des Einflusses von Probenmatrices werden dargestellt und die Ergebnisse einiger Messkampagnen und Ringversuche vorgestellt, die die Routinefähigkeit des Verfahrens dokumentieren.
Die Vorgehensweise bei der Zertifizierung von Referenzmaterialien in der BAM entsprechend den Regeln des ISO-Guide 35 wird an Beispielen beschrieben. Darüber hinaus wird ein umfassender Überblick über Referenzmaterialien zur Analyse der Nichtmetalle Sauerstoff, Wasserstoff, Stickstoff, Kohle und Schwefel gegeben.
Perhaps due in no small part to its historical mystique, mechanochemistry has been shrowded in relative obscurity for quite some time. The successes of mechanochemistry in organic synthesis have often been curtailed by a fundamentally limited mechanistic understanding. Lately, however, the community has made great strides towards understanding the fundamentals, as well as large steps forward regarding industrially significant scale-up via twin-screw extrusion. A variety of recent work has traded in some of mechanochemistry’s mystique for simple, straight-forward chemical guidelines.