Chemie und Prozesstechnik
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Zellen, als Grundeinheit für Organismen, bilden einen wesentlichen Eckpfeiler für das Leben. Die Untersuchung von einzelnen Zellen liefert wertvolle Einblicke in fundamentale Prozesse des Lebens. So können Anomalien auf der Zelleebene Indikatoren für Krankheiten sein und durch eine Analyse früh erkannt werden. Weiterhin kann durch ein tiefgreifendes Verständnis von Vorgängen in Zellen auch gezielt Forschung zu z.B. neuen Medikamenten betrieben werden. Damit können die Wirksamkeit erhöht und die Nebenwirkungen reduziert werden.
Materials in contact with the environment release e.g., metal-ions, elemental species and/or (nano-)particles. Once these species and/or particles are released, they are ingested by organisms and cells and thus, might have a negative impact on the environment. Thus, identification as well as quantification of potentially harmful substances is of utmost importance and highly needed to assess ecotoxicological impact of (emerging) pollutants.
The oral presentation provides an overview on the power of elemental analytical techniques, in particular ICP-MS as well as HR-CS-GFMAS in environmental research. Current research topics from Division 1.1 @ BAM - Inorganic trace analysis will be highlighted:
i) Elemental Speciation & Isotope analysis - new tools:
Among elemental species separation and quantification, one of the main challenges in environmental elemental speciation analysis is the distinction between anthropogenic and natural elemental species. The on-line combination of elemental speciation and isotope analysis combines “the best from both worlds” - species specific isotopic information becomes available.
As an application example the analysis of current anti-fouling agents via CE/MCICP-MS will be highlighted.
ii) HR-CS-GFMAS for PFC analysis:
Per- and polyfluorinated compounds (PFC) are emerging contaminants in particular in soil and surface water samples. Due to the large number of compounds (>4700), target analytical methods are not sufficient and sum parameter methods for organically bound fluorine are highly needed.
High resolution-continuum source-graphite furnace molecular absorption spectroscopy (HR-CS-GFMAS) based methods for organically bound fluorine analysis will be presented. Application examples (soil and surface water) will be highlighted.
iii) Single cell-ICP-ToF-MS - ecotox. assessment:
Single cell and single organism analysis for e.g. ecotoxicological/medicinal assessment are hot topics in the research field of ICP-MS. In particular ICP-ToF-MS is a powerful, emerging techniques in terms of single cell/particle analysis.
Automated single cell/diatom-ICP-ToF-MS as a potential tool in ecotoxicological testing will be presented.
With the latest ICP-MS technology - ICP-ToF (time of flight)-MS - it is possible to analyze the multi-element fingerprint of individual cells. The interface between material and environmental analysis thus receives special attention, e.g. when considering corrosion processes. Microbiologically influenced corrosion (MIC) is highly unpredictable due to the diversity of microbial communities involved. The development of the MIC-specific ICP-ToF-MS analytical method presented here at the single cell level, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis and will enable clarification of the processes taking place.
The supplied document shows the basis of a four minutes lightning talk.
Per- und polyfluorierte Alkylverbindungen (PFAS) sind sehr persistent und reichern sich in der Umwelt und im menschlichen Organismus in immer höheren Konzentrationen an. PFAS stellen deshalb eine große Gefährdung für Mensch und Umwelt dar. Eingesetzt werden sie u. a. als wasser- und fettabweisende Beschichtung in z. B. der Papier- und Textilindustrie und gelangen so während Produktion, Gebrauch und Entsorgung u. a. in den Wasserkreislauf. PFAS konnten sogar in der arktischen Umwelt in relevanten Konzentrationen detektiert werden und zählen somit zu den „emerging pollutants“. Ein prominenter Vertreter der PFAS stellt Perfluoroctansulfonsäure (PFOS) dar - die jedoch bereits im Anhang des Stockholmer Abkommen gelistet wurde und deren Einsatz somit stark eingeschränkt bzw. verboten ist. Im Hinblick auf die Vielzahl von Verbindungen werden neue analytische Methoden benötigt, die eine PFAS-Belastungssituation möglichst umfassend und nachweisstark widerspiegeln, um zukünftig mögliche Grenzwerte ableiten zu können.
In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement.
In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species using a multiple-injection approach for instrumental mass bias correction by standard-sample bracketing. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared to data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was promising regarding the differentiation of the river systems by the isotopic signature of river water sulfate. The great potential of this method is based on the versatility of the applied separation technique, not only in the environmental field but also for, e.g., biomolecules, as sulfur is the only covalently bound constituent of proteins that can be analyzed by MC-ICP-MS.
ICP-ToF (Flugzeitanalysator, engl. time of flight)-MS ermöglicht den Multielement Fingerabdruck einzelner Zellen (single cell) zu analysieren. Die single cell-ICP-ToF-MS kommt bei dem vorgestellten Poster bei der Analyse von Archaeen, die an mikrobiell beeinflusster Korrosion (engl. microbiologically influenced corrosion, MIC) von Stahl eine Rolle spielen, zum Einsatz. Mittels sc-ICP-ToF-MS wird die mögliche Aufnahme von einzelnen Elementen aus dem jeweiligen Stahl untersucht – die erhaltenen Informationen fließen zukünftig in die Aufklärung zugrunde liegender Mechanismen sowie Entwicklung möglicher Materialschutzkonzepte ein. Die Arbeiten Verknüpfen moderne Methoden der Analytical Sciences mit Materialien.
Molekülmassenspektrometrie entwickelt sich weg von klassischer Target- hin zu Nontarget-Analytik. Elementmassenspektrometrie liefert hohe Ortsauflösung beim Element-Imaging und analysiert einzelne Zellen. Aufgrund der Fortschritte bei den Geräten für Timeof-Flight-Massenspektrometrie mit induktiv gekoppeltem Plasma (ICPToF-MS) lässt sich das gesamte Periodensystem der Elemente in kurzen transienten Signalen quasi-simultan massenspektrometrisch erfassen.
Nearly all disease processes are associated with variations of components of the extracellular matrix (ECM) that are typically observed during the development of inflammation. This concerns for example proteoglycans and their associated glycosaminoglycans (GAG), which have been shown to bind to cationic metal imaging probes due to their strong complexing activity. The complexing activity largely depends on the degree of GAG sulfation and/or carboxylation as well as on the GAG isomericity. In this central project, we investigate GAG structures from inflammatory disorders (namely cardiovascular diseases, inflammatory intestinal diseases and neuroinflammation) provided by researchers of the Collaborative Research Center at the molecular disaccharidic level using chromatographic and mass spectrometric methods. In parallel, the spatial localization and quantification of metal-based imaging probes are evaluated by LA-ICP-MS imaging.
Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse mit über 5200 Verbindungen. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“. Die PFAS-Analytik ist wegen den 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. Weiterhin wird die Analytik aufgrund der Substitution von bereits regulierten PFAS mit ständig steigenden Anzahlen an PFAS-Verbindungen in der Umwelt konfrontiert. PFAS-Summenparameter-Methoden, die ein nahezu vollständiges Abbild der PFAS-Belastungssituation wiedergeben, werden daher immer wichtiger. In unserer Studie haben wir die zwei meistverwendeten PFAS-Summenparameter, das adsorbierbare organisch gebundene Fluor (AOF) und das extrahierbare organisch gebundene Fluor (EOF), miteinander verglichen. Beide Summenparameter können zur Analyse mit entweder combustion-Ionenchromatographie (CIC) oder hochauflösender Molekülabsorptionsspektrometrie (HR-CS-GFMAS) gekoppelt werden. Hierbei diskutieren wir die Vor- und Nachteile sowohl von beiden Summenparameter- als auch beider Detektions-Methoden. Die Untersuchungen wurden mit Oberflächenwasserproben aus der Spree in Berlin durchgeführt. Neben AOF und EOF wurde auch der Gesamt-Fluorgehalt (TF) mit CIC sowie HR-CS-GFMAS bestimmt. Die Fluor-Massenbilanzierung zeigte, dass das Verhältnis AOF/TF höher als das Verhältnis EOF/TF war. Dabei machte der AOF 0.14–0.81% vom TF und der EOF 0.04–0.28% vom TF aus. Insgesamt war die neue EOF/HR-CS-GFMAS-Methode schneller, präziser und sensitiver als die bereits etablierte AOF/CIC-Methode. Beide Methoden sind vielversprechend für die zukünftige Überwachung von Umweltproben und bilden die Grundlage für mögliche Grenzwerte, die auf die Summe PFAS abzielen.
In der Verbindungsklasse der per- und polyfluorierte alkylischen Substanzen (PFAS) werden über 5200 organische Verbindungen zusammengefasst. PFAS sind an mindestens einem Kohlenstoffatom vollständig fluoriert. Sie werden mit negativen Einflüssen auf die menschliche und tierische Gesundheit assoziiert, sind extrem persistent in der Umwelt und bioakkumulieren entlang von Nahrungsnetzen. Daher zählen PFAS zu den „emerging pollutants“. Gleichzeitig machen ihre physikalisch-chemischen Eigenschaften sie für die Verwendung in diversen technischen Anwendungen attraktiv. Sie sind sowohl hydro- als auch lipophob und zeigen durch die starke C-F-Bindung hohe thermische wie chemische Beständigkeit.
Erste Regulierungen einiger PFAS in Kombination mit den technisch hervorragenden Eigenschaften erzeugt einen Innovationsdruck und führten zu einem enormen Anstieg in der Zahl der Substitutionsverbindungen. Auf Grund der steigenden Komplexität der Substanzklasse ist die Target-Analytik nicht in der Lage eine solche Vielfalt und Vielzahl an Analyten zu erfassen.
Für eine akkurate Erfassung der Belastungssituation durch PFAS, die Identifikation von PFAS-Hotspots und eine Bewertung von geeigneten Sanierungsmaßnahmen ist daher eine geeignete PFAS-Summenparameteranalytik notwendig.
Daher geben wir hier Einblicke in den aktuellen Stand der PFAS-Summenparameterentwicklung und präsentieren unsere neusten Ergebnisse zur Methodenentwicklung für die quantitative Analyse von PFAS als extrahierbares organisch gebundenes Fluor (EOF) in Umweltproben mittels hochauflösender Molekülabsorptionsspektrometrie (HR-CS-GFMAS). Hierfür optimierten wir die Extraktion von PFAS aus verschieden Feststoff-Matrizes bei zeitgleicher Abtrennung anorganischen Fluorids. Durch den Zusatz von Galliumsalz-Lösungen als modifier in der HR-CS-GFMAS kann Fluor indirekt sehr selektiv durch die in situ Bildung von GaF sehr nachweisstark (instrumentelle LOQ ~3 µg/L) quantifiziert werden.
Since it is unknown for many applications, which PFASs are used and how they enter the environment, target analysis-based methods reach their limits. The two most frequently used sum parameters are the adsorbable organically bound fluorine (AOF) and the extractable organically bound fluorine (EOF). Both can be quantified using either combustion ion chromatography (CIC) or high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Here we provide an insight on the advantageous and disadvantageous of both sum parameters and both detection methods. Our study is based on the analysis of surface water samples. Next to total fluorine (TF) analysis, AOF and EOF were determined as well as CIC and HR-CS-GFMAS are compared and results are comparatively discussed. Fluorine mass balancing revealed that, the AOF/TF proportion was higher than the EOF/TF proportion. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF. Although, organically bound fluorine represents only a small portion of TF, PFASs are of worldwide concern, because of their extreme persistence and their bioaccumulation potential. The EOF-HR-CS-GFMAS method turned out to be more precise and sensitive than the AOF-CIC method and is a promising tool for future monitoring studies/routine analysis of PFASs in the environment.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is nowadays a versatile and powerful analytical method for direct solid sample analysis. The applicability has been demonstrated for a wide variety of samples covering hard and soft materials. In an imaging mode the technique provides quantitative information on the elemental distribution within a sample. LA-ICP-MS imaging is of particular interest in biomedical research as the distribution of an element gives valuable insight on uptake and distribution of essential and toxic trace elements, administered contrast agents as well es nanoparticles. LA-ICP-MS is therefore a powerful complement to other imaging techniques. Recent instrumental improvements, especially in sample chamber design, have contributed to better sensitivity and spatial resolution enabling subcellular imaging. The book chapter provides a comprehensive overview about spatially resolved localisation and quantification of various nanoparticles in cells and tissue thin sections by LA-ICP-MS. Furthermore, different sample preparation strategies and internal standardisation and calibration approaches for bioimaging by LA-ICP-MS are summarized and discussed.
Metal-containing nanomaterials are used in numerous fields ranging from industrial applications to nanomedicine. Several studies have demonstrated that the physicochemical properties of nanoparticles have an impact on their pharmacokinetics, transfer and clearance. The high sensitivity and multielement capability of LA-ICP-MS enables the elucidation of interactions between tissue components and nanomaterials used as imaging probes or drug carriers. Potential toxic effects are investigated as well. Thus, LA imaging significantly supports the clinical translation of safe and efficient nanoparticles for diagnostic and therapeutic purposes.
Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future.
Materials in contact with the environment release e.g., metal-ions, elemental species and/or (nano-)particles. Once these species and/or particles are released, they are ingested by organisms and cells and thus, might have a negative impact on the environment. Thus, identification as well as quantification of potentially harmful substances is of utmost importance and highly needed to assess ecotoxicological impact of (emerging) pollutants.
The oral presentation provides an overview on the power of elemental analytical techniques, in particular: ICP-MS as well as HR-CS-GFMAS in environmental research. Current research topics will be highlighted:
i) Elemental Speciation analysis of anti-fouling agents via CE/MC-ICP-MS;
ii) Per- and polyfluorinated compounds in surface waters via high resolution-continuum source-graphite furnace molecular absorption spectroscopy (HR-CS-GFMAS);
iii) Single cell and single organism analysis via sc-ICP-ToF-MS and ETV/ICP-MS for ecotoxicological assessment.
ICP-ToF (time of flight) MS enables the analysis of the multi-element fingerprint of single cells. The single cell ICP-ToF-MS is used in the presented poster for the analysis of archaea involved in microbiologically influenced corrosion (MIC) of steel. By means of sc-ICP-ToF-MS, the possible uptake of individual elements from the respective steel is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts. The work combines modern methods of analytical sciences with materials.
The latest ICP-MS technology - ICP-ToF (time of flight)-MS – enables the analysis of the multi-element fingerprint of individual cells. The interface between material and environmental analysis thus receives special attention, e.g., when considering corrosion processes. Microbiologically influenced corrosion (MIC) is a highly unpredictable phenomenon due to the influence of the environment, microbial communities involved and the respective electron source. However, the interaction pathway between cells and the metal surface remains unclear. The development of the MIC-specific ICP-ToF-MS analytical method presented here at the single cell level, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis and will enable clarification of the processes taking place. For this, a MIC-specific staining procedure was developed. It allows the analysis of archaea at a single cell level and provides information about the interaction of the cells with the staining agent which is extremely scarce compared to other well characterized organisms. Additionally, the single cell ICP-ToF-MS is used for the analysis of archaea involved in MIC of steel. Hence, the possible uptake of individual elements from different steel samples is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials.
Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future.