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Nicht zuletzt bedingt durch den Pferdefleischskandal im Jahr 2013 wurden in Deutschland die Aktivitäten bei der Methodenstandardisierung im Bereich der Tierarten-Differenzierung in den vergangenen Jahren intensiviert. Wenn auch positive Befunde bei dem Nachweis von Bestandteilen aus Pferd in Lebensmitteln wie Lasagne derzeit so gut wie nicht mehr anzutreffen sind, so hat die Tierartendifferenzierung insgesamt beim Nachweis von Verfälschungen in Lebensmitteln einen hohen Stellenwert.
Diese Arbeit fasst daher den aktuellen Stand der Analytik in Deutschland mit Schwerpunkt bei der Standardisierung zusammen. Sie wurde erstellt durch die Arbeitsgruppe „Biochemische und molekularbiologische Analytik“ der Lebensmittelchemischen Gesellschaft mit Unterstützung von Experten der Arbeitsgruppe „Molekularbiologische Methoden zur Pflanzen- und Tierartendifferenzierung“ (§ 64 LFGB) sowie der ALTS-Arbeitsgruppe „Immunologie und Molekularbiologie“ (jeweils D).
In the field of animal species differentiation, work on standardizing methods has been intensified in Germany in recent years, not least due to the horsemeat scandal in 2013. Even though there are now hardly ever any positive findings anymore in examinations to detect horse adulterations in foods such as lasagne, animal species differentiation altogether ranks high in detecting adulteration of foods. This article, therefore, summarises the current status of analytical techniques used in Germany with standardization at German level. It has been established by the working group "Biochemical and Molecular Biological Analytics" of the Lebensmittelchemische Gesellschaft (Food Chemistry Society within the German Chemical Society) with support of experts in the working group “Molecular biology techniques for differentiating plant and animal species" (§64 of the German Food and Feed Code - LFGB) and the "Immunology and molecular biology" task force of the food hygiene and food of animal origin working group (ALTS), both from Germany.
Work on standardising methods in the field of animal species differentiation has been intensified in Germany in recent years, not least due to the horsemeat scandal in 2013. Even though there are now hardly ever any positive findings any more in examinations to detect horse adulterations in foods such as lasagne, animal species differentiation altogether ranks high in detecting adulteration of foods. This article therefore summarises the current status of analytical techniques used in Germany with standardisation at German level. It has been established by the working group “Biochemical and Molecular Biological Analytics” of the Lebensmittelchemische Gesellschaft (Food Chemistry Society within the German Chemical Society) with support of experts in the working group “Molecular biology techniques for differentiating plant and animal species” (§ 64 of the German Food and Feed Code – LFGB) and the “Immunology and molecular biology” task force of the food hygiene and Food of animal origin working group (ALTS), both from Germany.
Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse bestehend aus mehreren tausenden Einzelverbindungen. Unter PFAS zählen alle Verbindungen, die mindestens eine perfluorierte Methyl- (-CF3) oder Methylen-Gruppe (-CF2-) besitzen. Somit zählt auch ein großer Teil der fluorierten Medikamente, Pflanzenschutzmittel oder Biozide in die PFAS-Substanzklasse. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“. Die PFAS-Analytik ist wegen ihrer vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. PFAS-Summenparameter-Methoden, die darauf abzielen ein möglichst vollständiges Abbild der PFAS-Belastungssituation widerzuspiegeln, werden daher immer wichtiger.
In this study, we compare analytical methods for PFAS determination–target analysis, non-target screening (NTS), direct total oxidizable precursor assay (dTOPA) and extractable organically bound fluorine (EOF). Therefore, suspended particulate matter (SPM) samples from German rivers at different locations in time series from2005 to 2020 were analyzed to investigate temporal and spatially resolved trends. In this study 3 PFAS mass balances approaches were utilized: (i) PFAA target vs. PFAS dTOPA, (ii) PFAS target vs. EOF and (iii) PFAS target vs. PFAS dTOPA vs. organofluorines NTS vs. EOF. Mass balance approach (i) revealed high proportions of precursor substances in SPM samples. For the time resolved analysis an increase from 94% (2005) to 97% in 2019 was observable. Also for the spatial resolved analysis precursor proportions were high with >84% at all sampling sites. Mass balance approach (ii) showed that the unidentified EOF (uEOF) fraction increased over time from82% (2005) to 99% (2019). Furthermore, along the river courses the uEOF increased. In the combined mass balance approach (iii) using 4 different analytical approaches EOF fractions were further unraveled. The EOF pattern was fully explainable at the sampling sites at Saar and Elbe rivers. For the time resolved analysis, an increased proportion of the EOF was now explainable. However, still 27% of the EOF for the time resolved analysis and 25% of the EOF for the spatial resolved analysis remained unknown. Therefore, in a complementary approach, both the EOF and dTOPA reveal unknown gaps in the PFAS mass balance and are valuable contributions to PFAS risk assessment. Further research is needed to identify organofluorines summarized in the EOF parameter.
The talk introduces the technique of LC-ELISA: fractionating pre-concentrated water samples, analyzing them for containing compounds that bind to hapten-selective antibodies followed by high-Resolution mass spectrometry non-target analysis of "positive" fractions for Transformation products of emerging organic contaminants.
For the first time, µ-X-ray fluorescence (µ-XRF) mapping combined with fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy was applied to depict per- and polyfluoroalkyl substances (PFAS) contamination and inorganic fluoride in samples concentrations down to 100 µg/kg fluoride. To demonstrate the matrix tolerance of the method, several PFAS contaminated soil and sludge samples as well as selected consumer product samples (textiles, food contact paper and permanent baking sheet) were investigated. µ-XRF mapping allows for a unique element-specific visualisation at the sample surface and enables localisation of fluorine containing compounds to a depth of 1 µm. Manually selected fluorine rich spots were subsequently analysed via fluorine K-edge µ-XANES spectroscopy. To support spectral interpretation with respect to inorganic and organic chemical distribution and compound class determination, linear combination (LC) fitting was applied to all recorded µ-XANES spectra. Complementarily, solvent extracts of all samples were target-analysed via LC-MS/MS spectrometry. The detected PFAS sum values range from 20 to 1136 µg/kg dry weight (dw). All environmentally exposed samples revealed higher concentration of PFAS with a chain length >C8 (e.g. 580 µg/kg dw PFOS for Soil1), whereas the consumer product samples showed a more uniform distribution with regard to chain lengths from C4 to C8. Independent from quantified PFAS amounts via target analysis, µ-XRF mapping combined with µ-XANES spectroscopy was successfully applied to detect both point-specific concentration maxima and evenly distributed surface coatings of fluorinated organic contaminants in the corresponding samples.
Wie können industriell synthetisierte Schadstoffe aus einer Stoffklasse quantifiziert werden, deren genauer Umfang unbekannt ist und auf mehrere tausend Verbindungen geschätzt wird? Im Falle der per- und polyfluorierten alkylierten Substanzen (PFAS) stellen sich Wissenschaftler*innen weltweit seit über zehn Jahren diese Frage. Neben der etablierten Methodik der Einzelstoffanalytik (engl. target analytic) existieren Summenparameteranalysen zur Quantifizierung
organisch gebundener fluorierter Verbindungen in Umweltmedien und Konsumprodukten. An der Bundesanstalt für Materialforschung und -prüfung (BAM) beschäftigen wir uns mit der Weiterentwicklung von Summenparametermethoden am Beispiel von PFAS-belasteten Umweltkompartimenten wie Böden, Klärschlämmen und Gewässerproben sowie PFAS-haltigen Konsumgütern. In diesem Beitrag stellen wir zwei ausgewählte Fallbeispiele vor und diskutieren die Vor- und Nachteile der Methoden im Vergleich zur Einzelstoffanalytik.
High-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) can be used for simultaneous quantification of various mycotoxins in contaminated food samples. Therefore, multi-mycotoxin methods have been developed in the last couple of years. To enlarge these methods for further analytes, we have developed a LC-MS/MS method for the quantification of the mycotoxin aurofusarin. Additionally, further LC-MSn experiments were performed to demonstrate the fragmentation pattern of aurofusarin. Applicable multiple reaction monitoring (MRM) transitions of aurofusarin were found and optimized by parameter variation of the tandem mass spectrometer. The applicability of the developed method was tested by analysis of naturally contaminated wheat.
An automated method is presented for fast simulation of (bio)transformation products (TPs) of the organophosphate insecticide chlorpyrifos CPF)based on electrochemistry coupled online to liquid chromatography-mass spectrometry (EC-LC-MS). Oxidative TPs were produced by a boron doped diamond (BDD) electrode, separated by reversed phase HPLC and online detected by electrospray ionization-mass spectrometry (ESI-MS). Furthermore, EC oxidative TPs were investigated by HPLC-tandem mass spectrometry (LC-MS/MS) and FT-ICR high resolution mass spectrometry (HRMS) and compared to in-vitro assay metabolites (rat and human liver microsomes). Main phase I metabolites of CPF: chlorpyrifos oxon (CPF oxon), trichloropyridinol (TCP), diethylthiophosphate (DETP), diethylphosphate (DEP), desethyl chlorpyrifos (De-CPF), and desethyl chlorpyrifos oxon (De-CPF oxon), were successfully identified by the developed EC-LC-MS method. The EC-LC-MS method showed similar metabolites compared to the in-vitro assay with possibilities of determining reactive species. Our results reveal that online EC-(LC)-MS brings an advantage on time of analysis by eliminating sample preparation steps and Matrix complexity compared to conventional in-vivo or in-vitro methods.