Chemische Charakterisierung und Spurenanalytik
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Paper des Monats
- ja (6)
This paper discusses the feasibility of a novel strategy based on the combination of bioprinting nano-doping technology and laser ablation-inductively coupled plasma time-of-flight mass spectrometry analysis for the preparation and characterization of gelatin- based multi-element calibration standards suitable for quantitative imaging. To achieve this, lanthanide up-conversion nanoparticles were added to a gelatin matrix to produce the bioprinted calibration standards. The features of this bioprinting approach were com- pared with manual cryosectioning standard preparation, in terms of throughput, between batch repeatability and elemental signal homogeneity at 5 μm spatial resolution. By using bioprinting, the between batch variability for three independent standards of the same concentration of 89 Y (range 0–600 mg/kg) was reduced to 5% compared to up to 27% for cryosectioning. On this basis, the relative standard deviation ( RSD ) obtained between three independent calibration slopes measured within 1 day also reduced from 16% (using cryosectioning ) to 5% (using bioprinting), supporting the use of a single standard preparation replicate for each of the concentrations to achieve good calibration performance using bioprinting. This helped reduce the analysis time by approximately 3-fold. With cryosectioning each standard was prepared and sectioned individually, whereas using bio-printing it was possible to have up to six different standards printed simultaneously, reducing the preparation time from approximately 2 h to under 20 min (by approxi- mately 6-fold). The bio-printed calibration standards were found stable for a period of 2 months when stored at ambient temperature and in the dark.
Over the last few years, the Federal Institute for material research (BAM, Berlin) together with the Centre for the Study of Manuscript Cultures (CSMC, University of Hamburg) have initiated a systematic material investigation of black inks produced from Late Antiquity to the Middle Ages (ca. fourth century CE–fourteenth/fifteenth centuries CE), aimed primarily at extending and complementing findings from previous sporadic studies. Part of this systematic investigation has focused on Egyptian Coptic manuscripts, and the present preliminary study is one of its outputs. It centres on a corpus of 45 Coptic manuscripts—43 papyri and 2 ostraca—preserved at the Palau-Ribes and Roca-Puig collections in Barcelona. The manuscripts come from the Monastery of Apa Apollo at Bawit, one of the largest monastic settlements in Egypt between the Late Antiquity and the Early Islamic Period (sixth–eighth centuries CE). The composition of their black inks was investigated in situ using near-infrared reflectography (NIRR) and X-ray fluorescence (XRF). The analyses determined that the manuscripts were written using different types of ink: pure carbon ink; carbon ink containing iron; mixed inks containing carbon, polyphenols and metallic elements; and iron-gall ink. The variety of inks used for the documentary texts seems to reflect the articulate administrative system of the monastery of Bawit. This study reveals that, in contrast to the documents, written mostly with carbon-based inks, literary biblical texts were written with iron-gall ink. The frequent reuse of papyrus paper for certain categories of documents may suggest that carbon-based inks were used for ephemeral manuscripts, since they were easy to erase by abrasion.
Amyloid fibrils are polymers formed by proteins under specific conditions and in many cases they are related to pathogenesis, such as Parkinson’s and Alzheimer’s diseases. Their hallmark is the presence of a β-sheet structure. High resolution structural data on these systems as well as information gathered from multiple complementary analytical techniques is needed, from both a fundamental and a pharmaceutical perspective. Here, a previously reported de novo designed, pH-switchable coiled coil-based peptide that undergoes structural transitions resulting in fibril formation under physiological conditions has been exhaustively characterized by transmission electron microscopy (TEM), cryo-TEM, atomic force microscopy (AFM), wide-angle X-ray scattering (WAXS) and solid-state NMR (ssNMR). Overall, a unique 2-dimensional carpet-like assembly composed of large coexisiting ribbon-like, tubular and funnel-like structures with a clearly resolved protofilament substructure is observed. Whereas electron microscopy and scattering data point somewhat more to a hairpin model of β-fibrils, ssNMR data obtained from samples with selectively labelled peptides are in agreement with both, hairpin structures and linear arrangements.
The calibration of isotope ratio measurements is an ongoing challenge since instrumental isotope fractionation (IIF) has been detected in mass spectrometry (MS). There is a variety of approaches which either bypass IIF such as delta measurements or refer to reference materials (RMs) and thus shifting the problem of calibration to somebody else: the RM producer. For certifying isotope RMs with absolute isotope ratios only a few approaches are available, namely the isotope mixture approach, the double spike approach, the mass bias regression model and total evaporation in TIMS. All of them require either enriched isotopes, isotope RMs of another element or an RM for correcting residual error. As the enriched isotopes required for the isotope mixture and the double spike approach need to be fully characterized beforehand, all mentioned calibration approaches require a standard.
Here, a new and standard-free calibration approach for obtaining absolute isotope ratios of multi-isotopic elements has been developed. The underlying principle is that each MS suffers from IIF and thus yields a specific isotope fractionation line in a three-isotope diagram. When applying a second MS featuring a different ionization mechanism, we obtain a second isotope fractionation line with a different slope in the same three-isotope diagram. In both cases the absolute isotope ratios range somewhere on the isotope fractionation line. Consequentially, the intersect of both lines yield the absolute isotope ratios of the measured sample. This theory has been tested by measuring Cd and Pb isotope ratios of suitable isotope RMs with a TIMS and an ICP-MS, both equipped with multi-collector array. During the measurements the ionization conditions were changed such that different extent of the isotope fractionation has been achieved. With the resulting data set the theory described above could be verified. The obtained absolute isotope ratios were metrologically compatible with the certified isotope ratios. The remaining average bias of -5 ‰ can be reduced with further improvements. The calibration approach is universal and can be applied to any multi-isotopic element and it is not limited by the type of the mass spectrometer.
The theory of a new calibration approach for obtaining absolute isotope ratios of multi-isotopic elements without the use of any standard has been developed. The calibration approach basically uses the difference in the instrumental isotope fractionation of two different types of mass spectrometers, leading to two different fractionation lines in a three-isotope diagram. When measuring the same sample with both mass spectrometers, the different fractionation lines have one point in common: this is the ‘true’ logarithmized isotope ratio pair of the sample. Thus, the intersection of both fractionation lines provides us with the absolute isotope ratios of the sample. This theory has been tested in practice by measuring Cd and of Pb isotope ratios in the certified reference materials BAM-I012 and NIST SRM981 by thermal ionization mass spectrometry and by inductively coupled plasma mass spectrometry while varying the ionization conditions for both mass spectrometers. With this experiment, the theory could be verified, and absolute isotope ratios were obtained, which were metrologically compatible with the certified isotope ratios. The so-obtained absolute isotope ratios are biased by − 0.5% in average, which should be improved with further developments of the method. This calibration approach is universal, as it can be applied to all elements with three or more isotopes and it is not limited to the type of mass spectrometers applied; it can be applied as well to secondary ion mass spectrometry or others. Additionally, this approach provides information on the fractionation process itself via the triple-isotope fractionation exponent θ.
The Uncertainty Paradox: Molar Mass of Enriched Versus Natural Silicon Used in the XRCD Method
(2020)
The X-ray crystal density method uses silicon spheres highly enriched in 28Si as a primary method for the dissemination of the SI base unit kilogram yielding smallest possible uncertainties associated with the mass m within a few parts in 10-8. This study compares different available and newly developed analytical methods and their results for the determination of the molar mass M of silicon highly enriched in 28Si (Me) and of silicon (Mx) with an almost natural isotopic distribution. While for Me relative uncertainties urel(Me) in the lower 10-9 range are obtained routinely, it was not possible to fall below a value of urel(Mx) < 4 x 10-6 in the case of natural silicon, which is approximately three orders of magnitude larger. The application of the state-of the-art isotope ratio mass spectrometry accompanied with sophisticated thoroughly investigated methods suggests an intrinsic cause for the large uncertainty associated with the molar mass of natural silicon compared to the enriched material.
Reference materials are essential, when the accuracy and reliability of measurement results need to be guaranteed in order to generate confidence in the analysis.
These materials are frequently used for determining measurement uncertainty, for validation of methods, suitability testing and quality assurance. Especially direct solid sampling methods require reference materials for calibration.
They guarantee that measurement results can be compared to recognized reference values.
This presentation gives an overview about the use of GDMS in various certification procedures. Because it represents a fast, sensitive, multielement analyses technique without extensive sample preparation it plays a special role for the purity determination of high purity standards. Various calibration strategies and the preparation of traceable matrix matched calibration standards will be discussed.
For the certification of analyte content in matrix materials mainly techniques with solvent sample preparation are used. Here GD-MS is used to identify possible loss or contamination with analytes during the sample preparation step. Typically used acids to dissolve matrices lead to interferences in the ICP- mass spectrometric detection of various analytes and their quantification. Here GD-MS as direct method can also add an important contribution in the certification process.
Glow discharge optical emission spectroscopy (GD-OES) is a technique for the analysis of solids such as metals, semiconductors, and ceramics. A low-pressure glow discharge plasma is applied in this system, which ‘sputters’ and promotes the sample atoms to a higher energy state. When the atoms return to their ground state, they emit light with characteristic wavelengths, which a spectrometer can detect. Thus, GD-OES combines the advantages of ICP-OES with solid sampling techniques, which enables it to determine the bulk elemental composition and depth profiles. However, direct solid sampling methods such as glow-discharge spectroscopy require reference materials for calibration due to the strong matrix effect.
Reference materials are essential when the accuracy and reliability of measurement results need to be guaranteed to generate confidence in the analysis. These materials are frequently used to determine measurement uncertainty, validate methods, suitability testing, and quality assurance. In addition, they guarantee that measurement results can be compared to recognized reference values. Unfortunately, the availability of certified reference materials suited to calibrate all elements in different matrix materials is limited. Therefore various calibration strategies and the preparation of traceable matrix-matched calibration standards will be discussed.
Machine learning is an essential component of the growing field of data science. Through statistical methods, algorithms are trained to make classifications or predictions, uncovering key insights within data mining projects. Therefore, it was tried in our work to combine GD-OES with machine learning strategies to establish a new and robust calibration model, which can be used to identify the elemental composition and concentration of metals from a single spectrum. For this purpose, copper reference materials from different manufacturers, which contain various impurity elements, were investigated using GD-OES. The obtained spectra information are evaluated with different algorithms (e.g., gradient boosting and artificial neural networks), and the results are compared and discussed in detail.
Thermal Destruction of PFAS
(2023)
Thermal treatment processes are currently the only full-scale option for thedestruction of per- and polyfluoroalkyl substances (PFAS) in large waste streams. While all organic molecules including PFAS are susceptible to thermal destruction, their decomposition rates are controlled by process variables such as temperature, reaction atmosphere, and residence time. Concerns exist about the formation of products of incomplete destruction and their emission from hazardous waste incinerators. This talk will summarize the current stateof-the-art of thermal PFAS destruction, identify research needs, and showcase future research designed to address critical knowledge gaps.
Thermo-Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to investigate the thermal degradation of two different polyurethanes (PU). PU samples were heated at different heating rates and the desorbed products were collected in a cold injection system and thereafter submitted to GC-MS. Prospects and limitations of the detection and quantification of semi-volatile degradation products were investigated. A temperature dependent PU depolymerization was
found at temperatures above 200 °C proved by an increasing release of 1,4-butanediol and methylene diphenyl diisocyanate (MDI) representing the main building blocks of both polymers. Their release was monitored quantitatively based on external calibration with authentic compounds. Size Exclusion Chromatography (SEC) of the residues obtained after thermodesorption confirmed the initial competitive degradation mechanism indicating an equilibrium of crosslinking and depolymerization as previously suggested. Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry of SEC fractions of thermally degraded PUs provided additional hints on degradation mechanism.
Besides conventional scanning X-ray fluorescence imaging at synchrotron sources, full-field X-ray fluorescence (FF-XRF) imaging techniques that do not implicitly require spatial scanning of the sample have become available. FF-XRF has become achievable thanks to the development of a new type of energy dispersive CCD-based 2D detector, also referred to as a 'color X-ray camera (CXC)' or 'SLcam'. We report on different imaging schemes for biological samples using FF-XRF imaging: (a) 2D 'zoom' imaging with pinhole optics using the 'camera obscura' principle; (b) 2D 'fixed magnification' imaging using magnifying polycapillary optics; and (c) 3D-FF-XRF imaging using an X-ray sheet beam or computed tomography (CT). The different FF-XRF imaging modes are illustrated using the crustacean Daphnia magna, a model organism for investigating the effects of metals on organism/ecosystem health, and foraminifera, a class of amoeboid protist. Detailed analytical characterization of the set-up is performed through analyzing various reference materials in order to determine limits of detection (LODs) and sensitivities. Experiments were performed using the BAMline at the BESSY synchrotron (Berlin, Germany) and using the P06 Hard X-ray Microprobe at the PETRAIII synchrotron (Hamburg, Germany).
In this study, a method for the determination of tire and road wear particle (TRWP) contents in particulate samples from road Environment was developed. Zn was identified as the most suitable elemental marker for TRWP, due to its high concentration in tire tread and the possibility of separation from other Zn sources. The mean concentration of 21 tire samples was 8.7 ± 2.0 mg Zn/g. Before quantification in samples from road environment, TRWP were separated from the particulate matrix by density separation. Method development was conducted using shredded tread particles (TP) as a surrogate for TRWP.
Recovery of TP from spiked sediment was 95 ± 17% in a concentration range of 2 - 200 mg TP/g. TP determination was not affected by other Zn containing solids or spiked Zn-salts. By adjusting the density of the separation solution to 1.9 g/cm3, more than 90% of total TRWP were separated from the sample matrix. TRWP concentrations in particulate matter collected in two road runoff treatment Systems ranged from 0.38 to 150 mg TRWP/g. Differences in quantified TRWP contents of the two Systems indicate changes in particle dynamics due to ageing and aggregation processes. The developed method allows TRWP determination in road runoff and in environments that are influenced by road traffic. The validated separation procedure can also be applied for TRWP characterization in future studies.
Given the central role of fatty acids in cancer pathophysiology, the exploitation of fatty acid metabolism as a potential antineoplastic therapy has gained much attention. Several natural and synthetic compounds targeting fatty acid metabolism were hitherto identified, and their effectiveness against cancer cell proliferation and survival was determined. This review will discuss the most clinically viable inhibitors or drugs targeting various proteins or enzymes mapped on nine interconnected fatty acid metabolism-related processes. We will discuss the general significance of each of these processes and the effects of their inhibition on cancer cell progression. Moreover, their mechanisms of action, limitations, and future perspectives will be assessed.
n situ monitoring of mechanochemical reactions between dicyandiamide (DCD) and CuX2 salts (X = Cl−, NO3−), for the preparation of compounds of agrochemical interest, showed the appearance of a number of phases. It is demonstrated that milling conditions, such as the amount of water added in wet grinding and/or the milling frequency, may affect the course of the mechanochemical reactions, and drive the reaction towards the formation of different products. It has been possible to discover by in situ monitored experiments two novel crystalline forms, namely the neutral complexes [Cu(DCD)2(OH2)2(NO3)2] (2) and [Cu(DCD)2(OH2)Cl2]·H2O (4), in addition to the previously known molecular salt [Cu(DCD)2(OH2)2][NO3]2·2H2O (1, DIVWAG) and neutral complex [Cu(DCD)2(OH2)Cl2] (3, AQCYCU), for which no synthesis conditions were available. Compounds 2 and 4 were fully characterized via a combination of solid-state techniques, including X-ray diffraction, Raman spectroscopy and TGA.
Matrix‐assisted ionization (MAI) mass spectrometry does not require voltages, a laser beam, or added heat to initiate ionization, but it is strongly dependent on the choice of matrix and the vacuum conditions. High charge state distributions of nonvolatile analyte ions produced by MAI suggest that the ionization mechanism may be similar to that of electrospray ionization (ESI), but different from matrix‐assisted laser desorption/ionization (MALDI). While significant information is available for MAI using mass spectrometers operating at atmospheric and intermediate pressure, little is known about the mechanism at high vacuum.
Eleven MAI matrices were studied on a high‐vacuum time‐of‐flight (TOF) mass spectrometer using a 266 nm pulsed laser beam under otherwise typical MALDI conditions. Detailed comparisons with the commonly used MALDI matrices and theoretical prediction were made for 3‐nitrobenzonitrile (3‐NBN), which is the only MAI matrix that works well in high vacuum when irradiated with a laser.
Screening of MAI matrices with good absorption at 266 nm but with various degrees of volatility and laser energies suggests that volatility and absorption at the laser wavelength may be necessary, but not sufficient, criteria to explain the formation of multiply charged analyte ions. 3‐NBN produces intact, highly charged ions of nonvolatile analytes in high‐vacuum TOF with the use of a laser, demonstrating that ESI‐like ions can be produced in high vacuum. Theoretical calculations and mass spectra suggest that thermally induced proton transfer, which is the major ionization mechanism in MALDI, is not important with the 3‐NBN matrix at 266 nm laser wavelength. 3‐NBN:analyte crystal morphology is, however, important in ion generation in high vacuum.
The 3‐NBN MAI matrix produces intact, highly charged ions of nonvolatile compounds in high‐vacuum TOF mass spectrometers with the aid of ablation and/or heating by laser irradiation, and shows a different ionization mechanism from that of typical MALDI matrices.
Analysis of single cells via LA-ICP-MS is a technique with great potential, however manual targeting of single cells is laborious and therefore microarraying of cells looks promising. In this work, we investigate the potential of a commercial non-contact piezo dispenser arraying system (S3, Scienion AG, Berlin), equipped with a novel technology for single-cell isolation called CellenONE™ (Cellenion, Lyon). Usually if one aims to create a microarray of single cells via spotting a suitably diluted cell suspension, one will observe a Poisson-distributed cell number per spot. CellenONE™ overcomes this problem by controlling the number of cells optically in the piezo dispense capillary (PDC) via image recognition to obtain true single cell arrays. The figures of merit of the customized and optimized setup will be presented. In a proof of concept experiment we investigated the trace elemental fingerprint of THP-1 cells by LA-ICP-TOF-MS (Analyte G2, Teledyne Cetac; icpTOF, TOFWERK) and quantified two metal cell dyes, mDOTA-Ho (CheMatech, Dijon), and Ir-DNA intercalator (Fluidigm, San Francisco). For that, matrix matched calibration standards after Wang et al. were successfully prepared using the same arraying system. We believe that this novel approach opens new ways for automated quantitative single cell LA-ICP-MS.
Towards Unbiased Evaluation of Ionization Performance in LC-HRMS Metabolomics Method Development
(2022)
As metabolomics increasingly finds its way from basic science into applied and regulatory environments, analytical demands on nontargeted mass spectrometric detection methods continue to rise. In addition to improved chemical comprehensiveness, current developments aim at enhanced robustness and repeatability to allow long-term, inter-study, and meta-analyses. Comprehensive metabolomics relies on electrospray ionization (ESI) as the most versatile ionization technique, and recent liquid chromatography-high resolution mass spectrometry (LC-HRMS) instrumentation continues to overcome technical limitations that have hindered the adoption of ESI for applications in the past. Still, developing and standardizing nontargeted ESI methods and instrumental setups remains costly in terms of time and required chemicals, as large panels of metabolite standards are needed to reflect biochemical diversity. In this paper, we investigated in how far a nontargeted pilot experiment, consisting only of a few measurements of a test sample dilution series and comprehensive statistical analysis, can replace conventional targeted evaluation procedures. To examine this potential, two instrumental ESI ion source setups were compared, reflecting a common scenario in practical method development. Two types of feature evaluations were performed, (a) summary statistics solely involving feature intensity values, and (b) analyses additionally including chemical interpretation.
Results were compared in detail to a targeted evaluation of a large metabolite standard panel. We reflect on the advantages and shortcomings of both strategies in the context of current harmonization initiatives in the metabolomics field.
To keep pace with the rising number of detected mycotoxins, there is a growing need for fast and reliable toxicity tests to assess the potential threat to food safety. Toxicity tests with the bacterial-feeding nematode Caenorhabditis elegans as model organism are well established. In this study the C. elegans wildtype strain N2 (var. Bristol) was used to investigate the toxic effects of the food-relevant mycotoxins citrinin (CIT) and zearalenone-14-sulfate (ZEA-14-S) and zearalenone (ZEA) on different life cycle parameters including reproduction, thermal and oxidative stress resistance and lifespan. The metabolization of the mycotoxins by the nematodes in vivo was investigated using HPLC-MS/MS. ZEA was metabolized in vivo to the reduced isomers α-zearalenol (α-ZEL) and β-ZEL. ZEA 14-S was reduced to α-/β-ZEL 14-sulfate and CIT was metabolized to mono-hydroxylated CIT. All mycotoxins tested led to a significant decrease in the number of nematode offspring produced. ZEA and CIT displayed negative effects on stress tolerance levels and for CIT an additional shortening of the mean lifespan was observed. In the case of ZEA-14-S, however, the mean lifespan was prolonged. The presented study shows the applicability of C. elegans for toxicity testing of emerging food mycotoxins for the purpose of assigning potential health threats.
Trace elements are chemical elements whose concentration in a material is very low. The exact definition depends on the application and varies for example between 100 micrograms per gram in analytical chemistry and 1000 micrograms per gram in geology. The ability to detect trace elements fast and quantitatively is of great importance in many areas of science and technology. With its high brilliance and flexibility in the excitation conditions, synchrotron radiation is an ideal tool for detecting traces even in small sample quantities. In this contribution I will report about the use of X-ray fluorescence(XRF)for qualitative and quantitative element sensitiveanalysis. In addition to the fundamentals of XRF and its quantification methods, the advantages and problems of different geometries like e.g. microXRF, Total Reflection X-ray Fluorescence (TXRF)or Double Dispersive XRF (D²XRF) will be discussed. Practical examples from BAMline from the research fields of medicine, geology and archaeometry will complete the lecture.
Data set of low-field NMR spectra of continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). 1H spectra (43 MHz) were recorded as single scans.
Two different approaches for the generation of artificial neural networks training data for the prediction of reactant concentrations were used: (i) Training data based on combinations of measured pure component spectra and (ii) Training data based on a spectral model.
Synthetic low-field NMR spectra
First 4 columns in MAT-files represent component areas of each reactant within the synthetic mixture spectrum.
Xi (“pure component spectra dataset”)
Xii (“spectral model dataset”)
Experimental low-field NMR spectra from MNDPA-Synthesis
This data set represents low-field NMR-spectra recorded during continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). Reference values from high-field NMR results are included.
Nebivolol (NEB), a β-blocker frequently used to treat cardiovascular diseases, has been widely detected in aquatic environments, and can be degraded under exposure to UV radiation, leading to the formation of certain transformation products (UV-TPs). Thus, the toxic effects of NEB and its UV-TPs on aquatic organisms are of great importance for aquatic ecosystems. In the present study, the degradation pathway of NEB under UV radiation was investigated. Subsequently, zebrafish embryos/larvae were used to assess the median lethal concentration (LC50) of NEB, and to clarify the sub-lethal effects of NEB and its UV-TPs for the first time. It was found that UV radiation could reduce the toxic effects of NEB on the early development of zebrafish. Transcriptomic analysis identified the top 20 enriched Kyoto Encyclopedia of Genes and Genomes (KEGG) pathways in zebrafish larvae exposed to NEB, most of which were associated with the antioxidant, nervous, and immune systems. The number of differentially expressed genes (DEGs) in the pathways were reduced after UV radiation. Furthermore, the analysis of protein biomarkers, including CAT and GST (antioxidant response), AChE and ACh (neurotoxicity), CRP and LYS (immune response), revealed that NEB exposure reduced the activity of these biomarkers, whereas UV radiation could alleviate the effects. The present study provides initial insights into the mechanisms underlying toxic effects of NEB and the detoxification effects of UV radiation on the early development of zebrafish. It highlights the necessity of considering the toxicity of UV-TPs when evaluating the toxicity of emerging pollutants in aquatic systems.
A poly(L-lactide) with a trifluoroethyl ester end group and an average degree of polymerization (DP) of 50 was synthesized by ROP of L-lactide initiated with trifluoroethanol. Small-angle X-ray scattering (SAXS) in combination with differential scanning calorimetry (DSC) measurements revealed an average crystal thickness of 13 nm, corresponding to 45 repeat units. This suggests that most crystallites were formed by extended PLA chains, and both flat surfaces were covered by CF3 groups. The crystalline PLAs were annealed at 140 or 160 °C in the presence of two catalysts: tin(II) 2-ethylhexanoate, (SnOct2) or dibutyltin bis(pentafluorophenoxide) (BuSnPhF). The chemical reactions, such as polycondensation and cyclization, proceeded in the solid state and were monitored by matrix-assisted laser desorption/ionization time-offlight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC) measurements. Under optimal conditions a large fraction of linear chains was transformed into crystallites composed of extended cycles. Additionally, MALDI TOF MS analysis of GPC fractions from samples annealed for 28 or 42 days detected chain elongation of the linear species up to a factor of 20.
For years there have been more and more reports on the presence of drugs in the aquatic environment. Due to the demographic change, the consumption of pharmaceuticals has risen sharply. After taking the drugs, they are partly metabolized in the human body. However, the metabolism is not complete so that both the metabolites and non-metabolized amounts of the parent compounds are excreted. These compounds reach the waste water and afterwards the sewage treatment plants. In sewage treatment plants transformation products can be formed by the oxidative conditions during wastewater treatment processes. The transformation products may have a higher toxicity than the actual environmental pollutants and are often only partly removed during the waste water treatment. Since a lot of these compounds are still unknown, the transformation products are not detected by target analysis used in sewage treatment plants and are often released undetected in the aquatic ecosystems. The released substances may be subject to additional transformation processes in the environment. Pharmaceuticals produced in high amounts can be already detected in the μg/L range in water bodies worldwide.
Metformin and its major transformation product guanylurea are one of the main representatives. Metformin is the drug of choice for treating type 2 diabetes. The drug therapy for diabetes mellitus has increased significantly in recent years. In the year 2015 1500 tons of metformin were prescribed in Germany (for statutory insured persons). Metformin is not metabolized in the human body and is excreted unchanged therefore concentrations between 57 μg/L and 129 μg/L are found in German waste water treatment plants influents.
In this work the transformation of the antidiabetic drug metformin is investigated. The degradation of metformin is initialize by commercial water treatment techniques like UV-radiation or noncommercial techniques like heterogenous photocatalysis based on titanium dioxide. The degradation of metformin and resulting transformation products are analyzed by LC-MS/MS and LC-HRMS.
The formation of transformation products (TPs) from contaminants and residues is becoming an increasing focus of scientific community. All organic compounds can form different TPs, thus demonstrating the complexity and interdisciplinarity of this topic. The properties of TPs could stand in relation to the unchanged substance or be more harmful and persistent. To get important information about the generated TPs, methods are needed to simulate natural and manmade transformation processes. Current tools are based on metabolism studies, photochemical methods, electrochemical methods, and Fenton's reagent. Finally, most transformation processes are based on redox reactions. This review aims to compare these methods for structurally different compounds. The groups of pesticides, pharmaceuticals, brominated flame retardants, and mycotoxins were selected as important residues/contaminants relating to their worldwide occurrence and impact to health, food, and environmental safety issues. Thus, there is an increasing need for investigation of transformation processes and identification of TPs by fast and reliable methods.
Zusätzlich zu Methodenentwicklung, Miniaturisierung und Kopplungsverfahren zeigen sich die Hyperspektroskopie zusammen mit Imaging‐Verfahren, der Einzelmolekülnachweis und der Einsatz von 3‐D‐Druckern als neue Schwerpunkte. Hinzu kommen künstliche Intelligenz bei Sensoren, Bildgebungsverfahren und Prozesssteuerung sowie die Vernetzung von Analyse‐ und Laborgeräten. Trends und Forschungsthemen aus der analytischen Chemie, zusammengestellt von elf Autoren, koordiniert von Günter Gauglitz.
For more than 110 years, BAM has been producing reference materials for a wide range of application fields. With the development of new analytical methods and new applications as well as continuously emerging more stringent requirements of laboratory accreditation with regard to quality control and metrological traceability, the demand and requirements for reference materials are increasing. This trend article gives an overview of general developments in the field of reference materials as well as developments in selected fields of application in which BAM is active. This includes inorganic and metal analysis, gas analysis, food and consumer products, and geological samples. In addition to these more traditional fields of application, developments in the areas of optical spectroscopy, particulary fluorescence methods, and nanomaterials are considered.
Trinamic TMCL IOC is a Python package designed for controlling stepper motors connected to a Trinamic board using the TMCL language (all boards supported by PyTrinamic should now work, has been tested on the TMCM 6110 and the TMCM 6214). Since it is implementing the TMCL protocol, it should be easy to adapt to other Trinamic motor controller boards. This package assumes the motor controller is connected over a machine network via a network-to-serial converter, but the underlying PyTrinamic package allows for other connections too.
This allows the control of attached motors via the EPICS Channel-Access virtual communications bus. If EPICS is not desired, plain Pythonic control via motion_control should also be possible. An example for this will be provided in the example.ipynb Jupyter notebook.
This package leverages Caproto for EPICS IOCs and a modified PyTrinamic library for the motor board control, and interfaces between the two via an internal set of dataclasses. Configuration for the motors and boards are loaded from YAML files (see tests/testdata/example_config.yaml).
The modifications to PyTrinamic involved extending their library with a socket interface. This was a minor modification that should eventually find its way into the official package (a pull request has been submitted).
In most chemical reactions, stable isotopes are fractionated in a mass-dependent manner, yielding correlated isotope ratios in elements with three or more stable isotopes. The proportionality between isotope ratios is set by the triple isotope fractionation exponent θ that can be determined precisely for, e.g., sulfur and oxygen by IRMS, but not for metal(loid) elements due to the lower precision of MC-ICP-MS analysis and smaller isotopic variations. Here, using Mg as a test case, we compute a complete metrologically robust uncertainty budget for apparent θ values and, with reference to this, present a new measurement Approach that reduces uncertainty on θ values by 30%. This approach, namely, direct educt-product bracketing (sample−sample bracketing), allows apparent θ values of metal(loid) isotopes to be determined precisely enough to distinguish slopes in three-isotope space. For the example of Mg, we assess appropriate quality Control standards for interference-to-signal ratios and Report apparent θ values of carbonate−seawater pairs. We determined apparent θ values for marine biogenic carbonates, where the foraminifera Globorotalia menardii yields 0.514 ± 0.005 (2 SD), the coral Porites, 0.515 ± 0.006 (2 SD), and two specimens of the giant clam Tridacna gigas, 0.508 ± 0.007 (2 SD) and 0.509 ± 0.006 (2 SD), documenting differences in the uptake pathway of Mg among marine calcifiers. The capability to measure apparent θ values more precisely adds a new dimension to metal(loid) δ values, with the potential to allow us to resolve different modes of fractionation in industrial and natural processes.
Analysis of microplastic particles (MP) in environmental samples needs sophisticated techniques and is time intensive due to sample preparation and detection. An alternative to the most common (micro ) spectroscopic techniques, FTIR or Raman spectroscopy, are the thermoanalytical methods, where specific decomposition products can be analyzed as marker compounds for different kind of plastics types and mass contents. Thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS) allows the fast identification and quantification of MP in environmental samples without sample preparation. Whereas up to now only the analysis of thermoplastic polymers was realized, this is the first time that even the analysis of tire wear (TW) content in environmental samples is possible. Various marker compounds for TW were identified. They include characteristic decomposition products of elastomers, antioxidants and vulcanization agents. Advantages and drawbacks of these marker substances were evaluated. Environmental samples from street run off were exemplarily investigated and presented.
Small organic molecule drugs are one of the key classes, taking increasingly important roles in modern drug development strategies. With the focus on small molecule drugs, difficulties originate frequently from a pronounced lipophilic character, resulting in poor water solubility, low bioavailability and unfavored pharmacokinetics. Recently, peptide-poly(ethylene glycol) conjugates (peptide-PEG conjugates) were described as precisely tunable platforms to solubilize a broad scope of fluorescent or non-fluorescent small organic molecules [1-2]. Selection of drug hosting peptides was achieved by combinatorial means, which can further be extended by implementation of a drug release screening step.
One-bead-one-compound peptide libraries are powerful tools to select high affinity binders. However, the selection of positive hits from the peptide libraries remains tedious as it occurs by handpicking, strongly limiting the pool of investigated beads. Here we report our recent results on improving the analytical platform, using automated fluorescence scanning and MALDI-ToF-ToF MS/MS imaging to screen larger sets of beads, broadening the statistical base and unraveling more precisely suitable peptides. The screening puts special emphasis on loading capacities and drug-release of transporters by performing additional washing steps in different media (cf. Fig. 1). Peptides representing strong, medium, weak releaser were chosen for further analysis and synthesized as peptide-polymer transporters. Release was analyzed by fluorescence anisotropy and fluorescence correlation spectroscopy, due to the fluorescent characteristics of the drug.
Solubilization studies confirmed sufficient loading capacities for a potential anti-Alzheimer disease drug of three transporter molecules representing strong/weak drug releaser, reaching solubilization of up to 1:3.4 (µmol drug/µmol conjugate). Fluorescence anisotropy and fluorescence correlation spectroscopy of the drug-loaded transporter showed significant differences in drug releasing properties, confirming the screening process.
Alternariol (AOH) and Alternariol monomethylether (AME) are two secondary metabolites of Alternaria fungi which can be found in various foodstuffs like tomatoes, nuts and grains. Due to their toxicity and potential mutagenic activity the need for the development of high-throughput methods for the supervision of AOH- and AME-levels is of increasing interest. As the availability of both native and labelled AOH and AME analytical standards is very limited we herein wish to present a novel concise approach towards their synthesis employing a ruthenium-catalyzed ortho-arylation4 as the key step.
In this work, the electrochemical behavior of 4-phenylurazole (Ph-Ur) was studied and the latter was used as a molecular anchor for the electrochemical bioconjugation of tyrosine (Y). Cyclic voltammetry (CV) and controlled potential coulometry (CPC) allowed the in-situ generation of the PTAD (4-phenyl-3 H-1,2,4-triazole-3,5(4 H)-dione) species from phenylurazole on demand for tyrosine electrolabeling. The chemoselectivity of the reaction was studied with another amino acid (lysine, Lys) and no changes in Lys were observed. To evaluate the performance of tyrosine electrolabeling, coulometric analyses at controlled potentials were performed on solutions of phenylurazole and the phenylurazole-tyrosine mixture in different proportions (2:1, 1:1, and 1:2). The electrolysis of the phenylurazole-tyrosine mixture in the ratio (1:2) produced a charge of 2.07 C, very close to the theoretical value (1.93 C), with high reaction kinetics, a result obtained here for the first time. The products obtained were identified and characterized by liquid chromatography coupled to high-resolution electrospray ionization mass spectrometry (LC-HRMS and LC- HRMS2). Two products were formed from the click reactions, one of which was the majority. Another part of this work was to study the electrochemical degradation of the molecular anchor 4-phenylazole (Ph-Ur). Four stable degradation products of phenylurazole were identified (C7H9N2O, C6H8N, C6H8NO, C14H13N4O2) based on chromatographic profiles and mass spectrometry results. The charge generated during the electrolysis of phenylurazole (two-electron process) (2.85 C) is inconsistent with the theoretical or calculated charge (1.93 C), indicating that secondary/parasitic reactions occurred during the electrolysis of the latter. In conclusion, the electrochemically promoted click phenylurazole-tyrosine reactions give rise to click products with high reaction kinetics and yields in the (1:2) phenylurazole-tyrosine ratios, and the presence of side reactions is likely to affect the yield of the click phenylurazole-tyrosine reaction.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is increasingly used to study the distribution of metal-containing drugs, imaging probes and nanomaterials in connection with disease related changes and therapy progress. Additionally, biomolecules can be detected indirectly by using metal-tagged antibodies.
The extracellular matrix (ECM) is, besides the cells, an important component of all body tissues. The macromolecular network of the ECM consists of structural proteins (e.g., collagen, elastin) and proteoglycans composed of highly negatively charged carbohydrates, the glycosaminoglycans (GAGs), which are covalently linked to a protein core. Many diseases, including inflammatory processes and tumors, are associated with characteristic ECM changes at an early stage. Recent studies have shown that contrast agents for magnetic resonance imaging (MRI), which are based on gadolinium containing chelate complexes or iron oxide nanoparticles, can bind themselves to ECM components.
To elucidate the role of GAGs like keratan sulfate (KS) and its modification state in disease, highly specific tools are necessary. As a complement to conventional immunohistochemistry LA-ICP-MS was applied to investigate the distribution of KS in tissue thin sections using a well characterized anti-KS antibody labelled with metal ions. Furthermore, LA-ICP-MS was used for the detection of MRI contrast agents and the identification of their target cells and molecules in tissue samples from animal models, e.g. for cardiovascular diseases. The results show the possibilities of LA-ICP-MS for the elucidation of pathological tissue changes.
Ionophore Antibiotika werden zum Schutz gegen Kokzidiose eingesetzt, hauptsächlich in der Geflügelmast. Rückstände dieser Substanzen und deren Transformationsprodukte (TP) gelangen über den Metabolismus zum einen in das Geflügelfleisch, aber auch durch Ausscheidung in die Umwelt, da Tiermist als Dünger verwendet wird. Ziel dieser Forschungsarbeit ist es, die TP-Bildung von vier verschiedenen Ionophoren Antibiotika (Monensin (MON), Salinomycin (SAL), Maduramicin (MAD) und Lasalocid (LAS)) zu untersuchen. TPs werden durch den Biotransformationsprozess (Metabolismus) gebildet, dieser Prozess kann in zwei Phasen eingeteilt werden. Während in Phase I Oxidations-, Reduktions- oder Hydrolysereaktionen auftreten, ist Phase II von Konjugationsreaktionen geprägt. Durch diesen Prozess werden die Substanzen besser ausscheidbar.
Natürliche Redox-Vorgänge, wie sie bei der Biotransformation (Phase I) auftreten, können mit elektrochemischen (EC) Systemen simuliert werden. In einer EC-Durchflusszelle findet die Reaktion abhängig vom angelegten Potential statt. Im positiven Potentialbereich (0.0 bis 3.0 V; vs. Pd/H2) werden die Analyten oxidiert und somit oxidative TPs generiert. Durch die online-Kopplung mit Flüssigkeitschromatografie (LC) und Massenspektrometrie (MS) wird zunächst eine säulenchromatografische Trennung der generierten TPs erhalten, gefolgt von der massenspektrometischen Detektion. Durch die online-Kopplung von EC-(LC)-MS ergibt sich eine schnelle Analysemöglichkeit von der TP-Erzeugung ausgewählter Substanzen bis hin zur Detektion, wodurch gleichzeitig eine Identifizierung möglich ist.
Die ausgewählten Ionophoren Antibiotika wurden mittels EC-(LC)-MS auf auftretende TPs untersucht. Die ersten Ergebnisse zeigen ein breites Spektrum unterschiedlicher TPs abhängig von gewählten EC-Parametern wie Lösemittel, Modifier und insbesondere vom Arbeitselektrodenmaterial der EC-Durchflusszelle. Unter den erhaltenen TPs sind sowohl bekannte als auch unbekannte TPs vertreten, so dass weitere Untersuchungen zur Strukturaufklärung und vergleichende Tests zu Phase I Metaboliten (z.B. durch Metabolismus-Studien mit Mikrosomen) geplant sind.
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 Berliner Sammlung "Manuscripta Americana" befinden sich Fragmente von Bilderhandschriften, die Alexander von Humboldt 1804 in Mexiko erwarb und der Königlichen Bibliothek schenkte. Die in der frühen Kolonialzeit hergestellten verschiedenartigen Codices waren damals schon nicht mehr an den Orten ihrer ursprünglichen Verwendung. Entsprechend ihres Seltenheitswertes gelangten einzelne Schriftstücke seit der Conquista in die Bestände bedeutender Persönlichkeiten. Hierzu fertigte man auch Abschriften oder Kopien an, oder zerstückelte sogar einzelne Blätter, so dass die Darstellungen auf den abgetrennten Fragmenten oft nur zum Teil abgebildet vorliegen.
Um herauszufinden, ob einige Schriftstücke der "Humboldt Codices" in Bezug zu einander stehen, werden die Dokumente, ihre Symbole und Schriftzeichen und das zur Herstellung verwendete Material miteinander verglichen.
Mit den für die Analyse von Manuskripten bewährten Untersuchungsmethoden werden Papier und Farbmittel identifiziert. Hierzu zählen Raman-, FTIR-, Röntgenfluoreszenz- und VIS- Spektroskopie. Charakteristisch für die Herstellung von schriftlichen Dokumenten in der Kolonialzeit von Amerika ist die Verwendung von indigenem Material wie Papier aus Baumrinde und Pflanzenfarben zusammen mit den aus Europa bekannten Materialien. Geklärt wird, inwieweit neben den bekanntesten Farbstoffen wie Cochenille, Mayablau oder Mischungen mit Tonmineralen auch mineralische Pigmente zum Einsatz kamen.
Vorgestellt werden die auf Tafel 36 in den "Vues des Cordillères et Monuments des Peuples Indigènes de l`Amerique, Voyage de Humboldt et Bonpland" abgebildeten Fragmente. Die hier von Humboldt vorgenommene Zusammenstellung wird mit der Farbpalette der in Berlin archivierten originalen Schriftstücke verglichen. Die Interpretation der Ergebnisse gibt einen Hinweis auf die Zuordnung oder auch Zusammengehörigkeit dieser einzigartigen Dokumente amerikanischer Geschichte. Hierbei wird die Frage aufgeworfen, inwiefern davon auszugehen ist, dass diese mit weiteren Fragmenten in Verbindung gebracht werden können, was für die Beleuchtung der kulturhistorischen Zusammenhänge von großer Bedeutung ist.
To keep up with emerging mycotoxins and their transformation products fast and reliable toxicity tests are needed. Toxicity testing of mycotoxins is carried out usually by performing in vitro assays or is evaluated by using laboratory animals like mice, rats or chicken in in vivo studies.
Settled between classical in vitro approaches and in vivo studies with higher animals are tests with the nematode Caenorhabditis elegans. Since Sydney Brenner described 1974 the cultivation and handling of C. elegans, this worm is widely used as model organism in developmental biology and neurology. Due to many benefits like easy and cheap cultivation, a completely sequenced genome and short generation time, it also plays an important role in toxicological research. Finally, the high number of conserved genes between human and C. elegans make the worm an ideal candidate for toxicological investigations.
In this study we used C. elegans to assess the toxic effects of the relevant food mycotoxin citrinin (CIT), the mycoestrogen zearalenone (ZEN) and the modified mycotoxin ZEN-14-sulfate (ZEN-14-S) on different lifetable parameters including reproduction, thermal and oxidative stress tolerance and lifespan. All tested mycotoxins significantly decreased the amount of offspring. In case of ZEN and CIT also significant negative effects on stress tolerance and lifespan were observed compared to the control group.
Moreover, metabolization of mycotoxins in the worms was investigated by using LC MS/MS. Extraction of the worms treated 5 days with mycotoxin-containing and UVC-killed bacteria showed metabolization of ZEN to α-ZEL and β-ZEL (ZEL = zearalenol, ratio about 3:2). ZEN 14-S was reduced to ZEL 14-S and CIT was metabolized to mono hydroxylated CIT.
Utilizing Aspergillus niger Fumonisin Amine Oxidase for the Electrochemical Detection of Fumonisin
(2023)
Fumonisins are a class of toxic secondary metabolites produced by various Fusarium species. The two most important producers of fumonisins are F. verticillioides and F. proliferatum but also Aspergillus niger is known to produce fumonisins. Most frequently they occur on maize, but also other grains can be contaminated with this group of mycotoxins. Exposure to fumonisins by dietary intake can have serious health effects on farm animals and also within humans. Thus, the European Commission sets legal limits for fumonisins in feed and foodstuffs. The detection of fumonisins is frequently performed in laboratories by chromatographic methods, which are costly and require trained personnel. Simplifying the analysis is therefore a major goal using portable detection systems. Electrochemical enzymatic biosensors offer great promise to meet this demand. Here we report for the first time an enzymatic fumonisin sensing approach with amperometric detection. For this purpose, an Aspergillus niger fumonisin amine oxidase (AnFAO) catalyzing the oxidative deamination of fumonisins, producing hydrogen peroxide, was recombinantly produced in E. coli. It was found that the specific activity of AnFAO using 20 μM Fumonisin B1 as substrate is higher than for 20 μM Fumonisin B2 with 0.122 U mg-1 and 0.058 U mg-1, respectively. It was possible to show a dependence of enzyme activity with enzyme – and substrate-concentration. For fumonisin B1 detection, the enzyme was coupled covalently to magnetic particles and the enzymatically produced H2O2 was detected amperometrically in a flow injection system using Prussian blue carbon electrodes. The developed method allows to quantify fumonisin B1 concentrations down to 1.5 µM and demonstrates that the recombinantly produced AnFAO was able to deaminate different concentrations of fumonisin even in immobilized form. Thus, this enzyme is well suited to develop an enzyme based electrochemical biosensor for fumonisin contaminated food and feed.
Draft standards for the determination of organic pollutants in the solid matter of environmental matrices such as sludge, treated biowaste and soil have been basically developed in the framework of the European standardization project HORIZONTAL. A research project financed by the German Federal Environment Agency was initiated to finalize some of these CEN standard drafts, since fully validated standard procedures are crucial for the evaluation of their reliability in the context of implementation in legislation on environmental health.
Approach: Appropriate test materials (< 2mm particle size) were prepared and homogenized from contaminated soils, sludge and treated biowaste containing polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), dioxins, furans and dioxin-like-PCB and served, along with reference solutions, as the basis for international interlaboratory comparisons. Performance data of three analytical standard procedures were obtained by the statistical evaluation of results received from 11 to 29 participants per test material.
Results: The overall variation coefficients of reproducibility (between-lab standard deviations) for the sum parameters were roughly between 10 and 35 %. The variation coefficients of repeatability (within-lab standard deviations) range between 3 % and 8 % and show no trend considering the substance groups or matrices.
The highest coefficients of reproducibility were found for the analysis of PAHs, which were between 26 and 35 %, depending on the matrix, whereas 7-17 % reproducibility was observed for toxicity equivalents (TEQ) comprising dioxins, furans and dl-PCB.
Conclusions: Overall, the results confirm that the procedures described in the Technical Specifications are fit for purpose for all three matrices and that the feasibility of the HORIZONTAL approach, to cover several matrices with one standard per analyte, was thereby proven.
The talk summarizes challenges in microplastic analysis. It shows the preparation of microplastic reference materials as well as the testing on homogeneity and stability. The reference material is used in an international laboratory comparison to compare different detection methods used for microplastic analysis. The methods used were µ-IR (FTIR+LDIR) for number-based methods and TED-GC/MS and Py-GC/MS for mass-based methods. The ILC was done under the umbrella of VAMAS TWA 45. Results of the participants are presented.
Vergleichende Darstellung SARS-CoV-2-spezifischer Nanobodys aus unterschiedlichen Wirtsorganismen
(2021)
Aufgrund der anhaltenden COVID-19-Pandemie werden neutralisierende Therapeutika benötigt. Eine Möglichkeit zur Behandlung stellt die Verwendung monoklonaler Anti-SARS-CoV-2-Immun-globuline dar. Ihre Produktion in Säugetierzellen ist jedoch schwer skalierbar, um den weltweiten Bedarf zu decken. VHH-Antikörper, auch Nanobodys genannt, bieten hierfür eine Alternative, da sie eine hohe Temperaturstabilität aufweisen und eine kostengünstige Produktion in prokaryotischen Wirtsorganismen ermöglichen.
Metal-containing nanoparticles (NP) can be characterized with inductively coupled plasma mass spectrometers (ICP-MS) in terms of their size and number concentration by using the single-particle mode of the instrument (spICP-MS). The accuracy of measurement depends on the setup, operational conditions of the instrument and specific parameters that are set by the user. The transport efficiency of the ICP-MS is crucial for the quantification of the NP and usually requires a reference material with homogenous size distribution and a known particle number concentration.
Currently, NP reference materials are available for only a few metals and in limited sizes. If particles are characterized without a reference standard, the results of both size and particle number may be biased. Therefore, a dual-inlet Setup for characterizing nanoparticles with spICP-MS was developed to overcome this problem. This setup is based on a conventional introduction system consisting of a pneumatic nebulizer (PN) for nanoparticle solutions and a microdroplet Generator (μDG) for ionic calibration solutions. A new and flexible interface was developed to facilitate the coupling of μDG, PN and the ICP-MS system. The interface consists of available laboratory components and allows for the calibration, nanoparticle (NP) characterization and cleaning of the arrangement, while the ICP-MS instrument is still running.
Three independent analysis modes are available for determining particle size and number concentration. Each mode is based on a different calibration principle.
While mode I (counting) and mode III (μDG) are known from the literature, mode II (sensitivity), is used to determine the transport efficiency by inorganic ionic Standard solutions only. It is independent of NP reference materials. The μDG based inlet system described here guarantees superior analyte sensitivities and, therefore, lower detection limits (LOD). The size dependent LODs achieved are less than 15 nm for all NP (Au, Ag, CeO2) investigated.