TY - JOUR
A1 - Hernandez-Castillo, A. O.
A1 - Bischoff, J.
A1 - Lee, J. H.
A1 - Langenhan, Jennifer
A1 - Karra, M.
A1 - Meijer, G.
A1 - Eibenberger-Arias, S.
T1 - High-resolution UV spectroscopy of 1-indanol
N2 - We report on rotationally resolved laser induced fluorescence (LIF) and vibrationally resolved resonanceenhanced multiphoton ionization (REMPI) spectroscopy of the chiral molecule 1-indanol. Spectra of the S1 ’ S0 electronic transition are recorded in a jet-cooled, pulsed molecular beam. Using two timedelayed pulsed lasers, the lifetimes of the S1 state of the two most stable conformers, referred to as eq1 and ax2, have been determined. The S1 ’ S0 origin bands of these conformers as well as the Transition to a vibrationally excited level in the S1 state of eq1 are recorded with full rotational resolution (25 MHz observed linewidth) by measuring the LIF intensity following excitation with a tuneable, narrowband cw laser. On selected rotationally resolved electronic transitions, Lamb-dips are measured to confirm the Lorentzian lifetime-contribution to the observed lineshapes. The rotationally resolved S1 ’ S0 origin band of a neon-complex of eq1 is measured via LIF as well. The fit of the rotationally resolved LIF spectra of the origin bands to those of an asymmetric rotor yields a standard deviation of about 6 MHz.
The resulting spectroscopic parameters are tabulated and compared to the outcome of ab initio calculations. For both conformers as well as for the Ne-eq1 complex, the geometric structures in the S0 and S1 states are discussed. For all systems, the transition dipole moment is mainly along the a-axis, the contributions along the b- and c-axes being about one order of magnitude smaller.
KW - REMPI
KW - LIF
KW - 1-indanol
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525056
DO - https://doi.org/10.1039/d0cp06170k
VL - 23
IS - 12
SP - 7048
EP - 7056
PB - Royal Society of Chemistry
AN - OPUS4-52505
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Herter, Sven-Oliver
A1 - Haase, Hajo
A1 - Koch, Matthias
T1 - Semisynthesis of Stable Isotope-Labeled Ergot Alkaloids for HPLC-MS/MS Analysis
N2 - Ergot alkaloids (EAs) are prevalent food contaminants affecting cereals, such as rye, wheat, and barley worldwide. To ensure EU safety standards, the six most common EAs: ergometrine, ergotamine, ergosine, ergocornine, ergocristine, and ergocryptine, and their epimers, are quantified using HPLC-MS/MS, as described in the European Standard Method EN 17425:2021. However, this can be challenging and time-consuming in food matrices without appropriate internal standards and highlights the need for more robust and precise analytical tools to support their monitoring. The development of isotope-labeled EAs directly addresses this gap, offering improved accuracy and leading to more consistency across laboratories and consequently to more consumer safety. Therefore, we developed a semisynthetic approach, building upon our previous work where native ergotamine was N6-demethylated to norergotamine and subsequently remethylated using iodomethane (13CD3-I). Herein, we are now able to present the successful synthesis of all of the isotopically labeled priority EAs. These isotope-labeled standards were tested against their native counterparts using HPLC coupled with HR-MS/MS. The chromatographic and mass spectrometric properties of the unlabeled and isotopically labeled EAs match exactly, confirming their successful synthesis and structure. These standards can now be utilized to enhance the accuracy and reliability of EA quantification in food and feed.
KW - Reference Material
KW - HPLC-MS/MS
KW - Mycotoxins
KW - Ergot Alkaloids
KW - Stable Isotope Dilution Analysis
KW - Semisynthesis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639692
DO - https://doi.org/10.1021/acs.jafc.5c03345
SN - 0021-8561
VL - 73
IS - 29
SP - 18412
EP - 18419
PB - American Chemical Society (ACS)
AN - OPUS4-63969
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Herter, Sven-Oliver
A1 - Koch, Matthias
A1 - Haase, Hajo
T1 - First Synthesis of Ergotamine-13CD3 and Ergotaminine-13CD3 from Unlabeled Ergotamine
N2 - Ergot alkaloids (EAs) formed by Claviceps fungi are one of the most common food contaminants worldwide, affecting cereals such as rye, wheat, and barley. To accurately determine the level of contamination and to monitor EAs maximum levels set by the European Union, the six most common EAs (so-called priority EAs) and their corresponding epimers are quantified using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The quantification of EAs in complex food matrices without appropriate internal tandards is challenging but currently carried out in the standard method EN 7425:2021 due to their commercial unavailability. To address the need for isotopically labeled EAs, we focus on two semi-synthetic approaches for the synthesis of these reference standards. Therefore, we investigate the feasibility of the N6-demethylation of native ergotamine to yield norergotamine, which can subsequently be remethylated with an isotopically labeled methylating reagent, such as iodomethane (13CD3-I), to yield isotopically labeled ergotamine and its C8-epimer ergotaminine. Testing the isotopically labeled ergotamine/-inine against native ergotamine/-inine with HPLC coupled to high-resolution HR-MS/MS proved the structure of ergotamine-13CD3 and ergotaminine-13CD3. Thus, for the first time, we can describe their synthesis from unlabeled, native ergotamine. Furthermore, this approach is promising as a universal way to synthesize other isotopically labeled EAs.
KW - Reference Material
KW - HPLC-MS/MS
KW - Mycotoxins
KW - Standards
KW - Organic Synthesis
KW - Isotope
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600167
DO - https://doi.org/10.3390/toxins16040199
VL - 16
IS - 4
SP - 1
EP - 12
PB - MDPI
AN - OPUS4-60016
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hildebrandt, L.
A1 - von der Au, Marcus
A1 - Zimmermann, T.
A1 - Reese, A.
A1 - Ludwig, J.
A1 - Pröfrock, D.
T1 - A metrologically traceable protocol for the quantification of trace metals in different types of microplastic
N2 - The presence of microplastic (MP) particles in aquatic environments raised concern About possible enrichment of organic and inorganic pollutants due to their specific surface and chemical properties. In particular the role of metals within this context is still poorly understood. Therefore, the aim of this work was to develop a fully validated acid digestion protocol for metal analysis in different polymers, which is a prerequisite to study such interactions.
The proposed digestion protocol was validated using six different certified reference materials in the microplastic size range consisting of polyethylene, polypropylene, acrylonitrile butadiene styrene and polyvinyl chloride. As ICP-MS/MS enabled time-efficient, sensitive and robust analysis of 56 metals in one measurement, the method was suitable to provide mass fractions for a multitude of other elements beside the certified ones (As, Cd, Cr, Hg, Pb, Sb, Sn and Zn). Three different microwaves, different acid mixtures as well as different temperatures in combination with different hold times were tested for optimization purposes.
With the exception of Cr in acrylonitrile butadiene styrene, recovery rates obtained using the optimized protocol for all six certified reference materials fell within a range from 95.9% ± 2.7% to 112% ± 7%. Subsequent optimization further enhanced both precision and recoveries ranging from 103% ± 5% to 107 ± 4% (U; k = 2 (n = 3)) for all certified metals (incl. Cr) in acrylonitrile butadiene styrene. The results clearly show the analytical challenges that come along with metal analysis in chemically resistant plastics. Addressing specific analysis Tools for different sorption scenarios and processes as well as the underlying kinetics was beyond this study’s scope. However, the future application of the two recommended thoroughly validated total acid digestion protocols as a first step in the direction of harmonization of metal analysis in/on MP will enhance the significance and comparability of the generated data. It will contribute to a better understanding of the role of MP as vector for trace metals in the environment.
KW - Microplatic
KW - Digestion
KW - Analytical Chemistry
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510727
DO - https://doi.org/10.1371/journal.pone.0236120
VL - 15
IS - 7
SP - e0236120
AN - OPUS4-51072
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hoffmann, A.
A1 - Lischeid, G.
A1 - Koch, Matthias
A1 - Lentzsch, P.
A1 - Sommerfeld, Thomas
A1 - Müller, M.H.
T1 - Co-Cultivation of Fusarium, Alternaria, and Pseudomonas on Wheat-Ears Affects Microbial Growth and Mycotoxin Production
N2 - Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads.
Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria enuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9).
Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies.
KW - Antagonists
KW - Microbe interactions
KW - Mycotoxins
KW - Priority effect
KW - SOM-SM
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521554
DO - https://doi.org/10.3390/microorganisms9020443
VL - 9
IS - 2
SP - 443
PB - MDPI
AN - OPUS4-52155
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hoffmann, Katrin
A1 - Nirmalananthan-Budau, Nithiya
A1 - Resch-Genger, Ute
T1 - Fluorescence calibration standards made from broadband emitters encapsulated in polymer beads for fluorescence microscopy and flow cytometry
N2 - We present here the design and characterization of a set of spectral calibration beads. These calibration beads are intended for the determination and regular control of the spectral characteristics of fluorescence microscopes and other fluorescence measuring devices for the readout of bead-based assays. This set consists of micrometer-sized polymer beads loaded with dyes from the liquid Calibration Kit Spectral Fluorescence Standards developed and certified by BAM for the wavelength-dependent Determination of the spectral responsivity of fluorescencemeasuring devices like spectrofluorometers. To cover the wavelength Region from 400 to 800 nm, two new near-infrared emissive dyes were included, which were spectroscopically characterized in solution and encapsulated in the beads. The resulting set of beads presents the first step towards a new platform of spectral calibration beads for the determination of the spectral characteristics of fluorescence instruments like fluorescence microscopes, FCM setups, and microtiter plate readers, thereby meeting the increasing demand for reliable and comparable fluorescence data especially in strongly regulated areas, e.g., medical diagnostics. This will eventually provide the basis for standardized calibration procedures for imaging systems as an alternative to microchannel slides containing dye solutions previously reported by us.
KW - Fluorescence standard
KW - Fluorescence
KW - Dye
KW - Microscopy
KW - Bead
KW - Particle
KW - NIR
KW - calibration
KW - Quality assurance
KW - Traceability
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508117
DO - https://doi.org/10.1007/s00216-020-02664-y
SN - 1618-2642
VL - 412
IS - 24
SP - 6499
EP - 6507
PB - Springer
AN - OPUS4-50811
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Homann, Christian
A1 - Peeters, Régis
A1 - Mirmajidi, Hana
A1 - Berg, Jessica
A1 - Fay, Michael
A1 - Rodrigues, Lucas Carvalho Veloso
A1 - Radicchi, Eros
A1 - Jain, Akhil
A1 - Speghini, Adolfo
A1 - Hemmer, Eva
T1 - Rapid microwave-assisted synthesis of morphology-controlled luminescent lanthanide-doped Gd2O2S nanostructures
N2 - Gadolinium oxysulfide (Gd2O2S) is an attractive material of demonstrated suitability for a variety of imaging applications, leveraging its magnetic, scintillating, and luminescent properties, particularly when doped with optically active lanthanide ions (Ln3+). For many of these applications, control over size and morphology at the nanoscale is crucial. This study demonstrates the rapid microwave-assisted Synthesis of colloidal Ln2O2S (Ln = Gd and dopants Yb, Er, Tb) nanostructures in as little as 20 min. Structural characterization using X-ray diffraction analysis (XRD), Raman spectroscopy, as well as Transmission electron microscopy (TEM), including elemental mapping via energy dispersive X-ray spectroscopy (EDS), unveiled the key role of elemental sulphur (S8) in the reaction mixtures for materials growth. By systematically varying the Ln-to-S ratio from 1 : 0.5 to 1 : 15, controlled morphologies ranging from triangular nanoplatelets to berry- and flower-like shapes were achieved. Doping with Er3+/Yb3+ endowed the nano-triangles with upconverting and near-infrared emitting properties. Tb3+-doped Gd2O2S exhibited the characteristic green Tb3+ emission under UV excitation, while also showing X-ray excited optical luminescence (XEOL), rendering the material interesting as a potential nano-scintillator.
KW - Upconversion
KW - Microwave-assisted synthesis
KW - Synthesis
KW - Fluorescence
KW - Nano
KW - Particle
KW - NIR
KW - XRD
KW - X-ray fluoressence
KW - Morphology control
KW - Raman
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647907
DO - https://doi.org/10.1039/D5TC01646K
SN - 2050-7526
VL - 13
IS - 35
SP - 18492
EP - 18507
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64790
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Horf, M.
A1 - Gebbers, R.
A1 - Vogel, S.
A1 - Ostermann, Markus
A1 - Piepel, M.-F.
A1 - Olfs, H.-W.
T1 - Determination of Nutrients in Liquid Manures and Biogas Digestates by Portable Energy-Dispersive X-ray Fluorescence Spectrometry
N2 - Knowing the exact nutrient composition of organic fertilizers is a prerequisite for their appropriate application to improve yield and to avoid environmental pollution by over-fertilization.
Traditional standard chemical analysis is cost and time-consuming and thus it is unsuitable for a rapid analysis before manure application. As a possible alternative, a handheld X-ray fluorescence (XRF) spectrometer was tested to enable a fast, simultaneous, and on-site analysis of several elements.
A set of 62 liquid pig and cattle manures as well as biogas digestates were collected, intensively homogenized and analysed for the macro plant nutrients phosphorus, potassium, magnesium, calcium, and sulphur as well as the micro nutrients manganese, iron, copper, and zinc using the standard lab procedure. The effect of four different sample preparation steps (original, dried, filtered, and dried filter residues) on XRF measurement accuracy was examined. Therefore, XRF results were correlated with values of the reference analysis. The best R2 s for each element ranged from 0.64 to 0.92. Comparing the four preparation steps, XRF results for dried samples showed good correlations (0.64 and 0.86) for all elements. XRF measurements using dried filter residues showed also good correlations with R2 s between 0.65 and 0.91 except for P, Mg, and Ca. In contrast, correlation Analysis for liquid samples (original and filtered) resulted in lower R2 s from 0.02 to 0.68, except for K (0.83 and 0.87, respectively). Based on these results, it can be concluded that handheld XRF is a promising measuring system for element analysis in manures and digestates.
KW - XRF
KW - Animal slurry
KW - Fertilizer
KW - Soil
KW - Precision farming
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527622
DO - https://doi.org/10.3390/s21113892
VL - 21
IS - 11
SP - 3892
PB - MDPI
CY - Basel, Switzerland
AN - OPUS4-52762
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hudson, A.D.
A1 - Jamieson, O.
A1 - Crapnell, R.D.
A1 - Rurack, Knut
A1 - Soares, T.C.C.
A1 - Mecozzi, F.
A1 - Laude, A.
A1 - Gruber, J.
A1 - Novakovic, K.
A1 - Peeters, M.
T1 - Dual detection of nafcillin using a molecularly imprinted polymer-based platform coupled to thermal and fluorescence read-out
N2 - Reported here is the production of molecularly imprinted polymer (MIP) films, integrating a fluorescent moiety that serves as both an element for template interaction and signalling, for the thermal and optical detection of the beta-lactam antibiotic nafcillin. Fluorescein methacrylate (FluMa) was synthesized and introduced during the molecular imprinting process as the sole monomer and in a 1 : 1 mixture with methacrylic acid (MAA), allowing to draw first conclusions on the MIP formation potential of such a rather large and rigid monomer. At first, MIP microparticles containing FluMa were prepared by free radical polymerisation. Optical batch rebinding experiments revealed that FluMa can act as a functional monomer for selective detection of nafcillin; however, the addition of MAA as co-monomer significantly improved performance. Subsequently, thin MIP films containing FluMa were deposited onto functionalised glass slides and the influence of porogen, drying time, and monomer composition was studied. These MIP-functionalised glass electrodes were mounted into a customised 3D-printed flow cell, where changes in the liquid were either evaluated with a thermal device or using fluorescence bright field microscopy. Thermal analysis demonstrated that multiple MIP layers enhanced sensor specificity, with detection in the environmentally relevant range. The fluorescence bright field microscope investigations validated these results, showing an increase in the fluorescence intensity upon exposure of the MIP-functionalised glass slides to nafcillin solutions. These are promising results for developing a portable sensor device that can be deployed for antibiotics outside of a dedicated laboratory environment, especially if sensor design and fluorophore architecture are optimised.
KW - Molecularly Imprinted Polymers
KW - Fluorescence
KW - Antibiotics
KW - Heat-transfer Measurements
KW - Thin films
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540044
DO - https://doi.org/10.1039/D1MA00192B
VL - 2
IS - 15
SP - 5105
EP - 5115
PB - Royal Society of Chemistry
CY - Cambridge
AN - OPUS4-54004
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hülagü, Deniz
A1 - Tobias, Charlie
A1 - Climent Terol, Estela
A1 - Gojani, Ardian
A1 - Rurack, Knut
A1 - Hodoroaba, Vasile-Dan
T1 - Generalized Analysis Approach of the Profile Roughness by Electron Microscopy with the Example of Hierarchically Grown Polystyrene–Iron Oxide–Silica Core–Shell–Shell Particles
N2 - The roughness as a property of core–shell (CS) microparticles plays a key role in their functionality. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task with approaches using electron microscopy images being scarce and showing pronounced differences in terms of methodology and results. This work presents a generalized method for the reliable roughness determination of nonplanar specimens such as CS particles from electron microscopic images, the method being robust and reproducible with a high accuracy. It involves a self-written software package (Python) that analyzes the recorded images, extracts corresponding data, and calculates the roughness based on the deviation of the identified contour. Images of single particles are taken by a dual mode scanning electron microscopy (SEM) setup which permits imaging of the same field-of-view of the sample with high resolution and surface sensitive in SE InLens mode as well as in transmission mode (TSEM). Herein, a new type of polystyrene core–iron oxide shell–silica shell particles is developed to serve as a set of lower micrometer-sized study objects with different surface roughness; the analysis of their images by the semiautomatic workflow is demonstrating that the particles’ profile roughness can be quantitatively obtained.
KW - Core–shell particles
KW - Image analysis
KW - Nanoparticles
KW - Roughness
KW - SEM
KW - transmission mode
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542576
DO - https://doi.org/10.1002/adem.202101344
SP - 1
EP - 9
PB - Wiley-VCH
AN - OPUS4-54257
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hülagü, Deniz
A1 - Tobias, Charlie
A1 - Dao, Radek
A1 - Komarov, Pavel
A1 - Rurack, Knut
A1 - Hodoroaba, Vasile-Dan
T1 - Towards 3D determination of the surface roughness of core–shell microparticles as a routine quality control procedure by scanning electron microscopy
N2 - AbstractRecently, we have developed an algorithm to quantitatively evaluate the roughness of spherical microparticles using scanning electron microscopy (SEM) images. The algorithm calculates the root-mean-squared profile roughness (RMS-RQ) of a single particle by analyzing the particle’s boundary. The information extracted from a single SEM image yields however only two-dimensional (2D) profile roughness data from the horizontal plane of a particle. The present study offers a practical procedure and the necessary software tools to gain quasi three-dimensional (3D) information from 2D particle contours recorded at different particle inclinations by tilting the sample (stage). This new approach was tested on a set of polystyrene core-iron oxide shell-silica shell particles as few micrometer-sized beads with different (tailored) surface roughness, providing the proof of principle that validates the applicability of the proposed method. SEM images of these particles were analyzed by the latest version of the developed algorithm, which allows to determine the analysis of particles in terms of roughness both within a batch and across the batches as a routine quality control procedure. A separate set of particles has been analyzed by atomic force microscopy (AFM) as a powerful complementary surface analysis technique integrated into SEM, and the roughness results have been compared.
KW - Core–shell particles
KW - Image analysis
KW - Roughness
KW - Scanning electron microscopy
KW - Atomic force microscopy
KW - Tilting
KW - Batch analysis
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607590
DO - https://doi.org/10.1038/s41598-024-68797-7
SN - 2045-2322
VL - 14
IS - 1
SP - 1
EP - 13
PB - Springer Science and Business Media LLC
AN - OPUS4-60759
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Inostroza, Manuel
A1 - Fernandez, Bárbara
A1 - Aguilera, Felipe
A1 - Layana, Susana
A1 - Walter, Thomas R.
A1 - Zimmer, Martin
A1 - Rodríguez-Díaz, Augusto
A1 - Oelze, Marcus
T1 - Physical and chemical characteristics of active sulfur flows observed at Lastarria volcano (northern Chile) in January 2019
N2 - Molten sulfur is found in various subaerial volcanoes. However, limited records of the pools and flows of molten sulfur have been reported: therefore, questions remain regarding the physicochemical processes behind this phenomenon. A suite of new sulfur flows, some of which active, was identified at the Lastarria volcano (northern Chile) and studied using satellite imagery, in situ probing, and temperature and video recording. This finding provides a unique opportunity to better understand the emplacement mechanisms and mineral and chemical compositions of molten sulfur, in addition to gaining insight into its origin. Molten sulfur presented temperatures of 124–158°C, with the most prolonged sulfur flow reaching 12 m from the source. Photogrammetric tools permitted the identification of levees and channel structures, with an estimated average flow speed of 0.069 m/s. Field measurements yielded a total volume of 1.45 ± 0.29 m3 of sulfur (equivalent to ∼2.07 tons) mobilized during the January 2019 event for at least 408 min. Solidified sulfur was composed of native sulfur with minor galena and arsenic- and iodine-bearing minerals. Trace element analysis indicated substantial enrichment of Bi, Sb, Sn, Cd, as well as a very high concentration of As (>40.000 ppm). The January 2019 molten sulfur manifestations in Lastarria appear to be more enriched in As compared to the worldwide known volcanoes with molten sulfur records, such as the Shiretoko-Iozan and Poás volcanoes. Furthermore, their rheological properties suggest that the “time of activity” in events such as this could be underestimated as flows in Lastarria have moved significantly slower than previously thought. The origin of molten sulfur is ascribed to the favorable S-rich chemistry of fumarolic gases and changes in host rock permeability (fracture opening). Molten sulfur in Lastarria correlates with a peak in activity characterized by high emissions of SO2 and other acid species, such as HF and HCl, in addition to ground deformation. Consequently, molten sulfur was framed within a period of volcanic unrest in Lastarria, triggered by changes in the magmatic-hydrothermal system. The appearance of molten sulfur is related to physicochemical perturbations inside the volcanic system and is perhaps a precursor of eruptive activity, as observed in the Poás and Turrialba volcanoes.
KW - General Earth and Planetary Sciences
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590331
DO - https://doi.org/10.3389/feart.2023.1197363
VL - 11
SP - 1
EP - 18
PB - Frontiers Media SA
AN - OPUS4-59033
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Jaeger, Carsten
A1 - Lintelmann, Jutta
A1 - Franke, Raimo
A1 - Artati, Anna
A1 - Cecil, Alexander
A1 - Broda, Frank
A1 - Klawonn, Frank
A1 - Erban, Alexander
A1 - Kopka, Joachim
A1 - Fuchs, Beate
A1 - Sommer, Ulf
A1 - Neumann-Schaal, Meina
A1 - O'Connor, Gavin
T1 - Analytical practices, use and needs of standard and reference materials in the German-speaking metabolomics community: results of an online survey
N2 - Introduction
Since the early 2000s, metabolomics has grown rapidly, becoming integral to fields like life sciences, health, and environmental research. This expansion has led to the formation of national and international societies, such as Germany’s DGMet, to tackle emerging challenges. One of DGMet’s goals is to improve measurement quality by assessing community needs for harmonization and standardization. A recent survey within the German-speaking community aimed to identify current practices and gaps in the use of chemical standards and reference materials, to guide future standardization efforts and collaborative initiatives.
Methods
An online survey was conducted between June 2023 and April 2024. The survey consisted of 38 key questions and was open to research institutions from Germany, Austria, and Switzerland.
Results
The survey was accessed by 68 laboratories, with 23 institutes providing complete or partial responses (34% response rate), which is comparable to rates reported in similar surveys within the metabolomics and lipidomics communities. Respondents were mainly experienced researchers from Germany, focusing mainly on health-related (“red”) metabolomics, as indicated by 78% of the respondents, followed by microbial (“grey”, 48%) and plant (“green”, 39%) metabolomics (multiple answers possible). The use of targeted methods was reported more frequently (91%) than that of non-targeted methods (78%), whereas metabolite fractions studied were equally split between polar, midpolar and lipid fractions (83% each). Human (74%), mouse (61%) and Arabidopsis (30%) were the most frequently studied organisms. Most participants used synthetic chemical standards for instrument qualification (83%), calibration (78%), and metabolite identification (74%), while matrix reference materials were mainly applied for quality control (52%) and method validation (44%). There was a strong demand for more standards, especially for metabolite identification and quantification, with cost being a major barrier, particularly for isotopically labelled standards and certified reference materials.
Conclusions
Valuable insights into the use of standards and reference materials within the German-speaking metabolomics community were obtained. Moving forward, the community should address critical gaps in metabolomics standardization. To achieve this, it must share its knowledge, articulate its needs clearly, and actively engage in joint efforts with national metrology institutes and international standardization initiatives.
KW - Reference material
KW - Chemical standard
KW - Metabolomics
KW - Mass spectrometry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647303
DO - https://doi.org/10.1007/s11306-025-02360-x
VL - 21
IS - 6
SP - 1
EP - 11
PB - Springer-Nature
CY - Heidelberg
AN - OPUS4-64730
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Jaeger, Carsten
A1 - Lisec, Jan
T1 - Towards Unbiased Evaluation of Ionization Performance in LC-HRMS Metabolomics Method Development
N2 - 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.
KW - Mass Spectrometry
KW - Non-targeted analysis
KW - Method development
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548065
DO - https://doi.org/10.3390/metabo12050426
VL - 12
IS - 5
SP - 1
EP - 13
PB - MDPI
AN - OPUS4-54806
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Jaeger, Carsten
A1 - Ritter, D.
A1 - Goeritzer, M.
A1 - Thiele, A.
A1 - Blumrich, A.
A1 - Beyhoff, N.
A1 - Luettges, K.
A1 - Smeir, E.
A1 - Kasch, J.
A1 - Grune, J.
A1 - Müller, O.
A1 - Klopfleisch, R.
A1 - Foryst-Ludwig, A.
A1 - Kintscher, U.
T1 - Liver X Receptor Agonist AZ876 Induces Beneficial Endogenous Cardiac Lipid Reprogramming and Protects Against Isoproterenol-Induced Cardiac Damage
N2 - Background - It is known that dietary intake of polyunsaturated fatty acids may improve cardiac function. However, relatively high daily doses are required to achieve sufficient cardiac concentrations of beneficial omega‐3 fatty acids. The liver X receptor (LXR) is a nuclear hormone receptor and a crucial regulator of lipid homeostasis in mammals. LXR activation has been shown to endogenously reprogram cellular lipid profiles toward increased polyunsaturated fatty acids levels. Here we studied whether LXR lipid reprogramming occurs in cardiac tissue and exerts cardioprotective actions.
Methods and Results - Male 129SV mice were treated with the LXR agonist AZ876 (20 µmol/kg per day) for 11 days. From day 6, the mice were injected with the nonselective β‐agonist isoproterenol for 4 consecutive days to induce diastolic dysfunction and subendocardial fibrosis while maintaining systolic function. Treatment with isoproterenol led to a marked impairment of global longitudinal strain and the E/e' ratio of transmitral flow to mitral annular velocity, which were both significantly improved by the LXR agonist. Histological examination showed a significant reduction in isoproterenol‐induced subendocardial fibrosis by AZ876. Analysis of the cardiac lipid composition by liquid chromatography‐high resolution mass spectrometry revealed a significant increase in cardiac polyunsaturated fatty acids levels and a significant reduction in saturated fatty acids by AZ876.
Conclusions - The present study provides evidence that the LXR agonist AZ876 prevents subendocardial damage, improves global longitudinal strain and E/e' in a mouse model of isoproterenol‐induced cardiac damage, accompanied by an upregulation of cardiac polyunsaturated fatty acids levels. Cardiac LXR activation and beneficial endogenous cardiac lipid reprogramming may provide a new therapeutic strategy in cardiac disease with diastolic dysfunction.
KW - Heart failure
KW - Lipids
KW - Liver X receptor
KW - Diastolic dysfunction
KW - Nuclear receptor
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529352
DO - https://doi.org/10.1161/JAHA.120.019473
VL - 10
IS - 14
SP - e019473
AN - OPUS4-52935
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Jiang, Shan
A1 - Wang, T.
A1 - Behren, S.
A1 - Westerlind, U.
A1 - Gawlitza, Kornelia
A1 - Persson, J. L.
A1 - Rurack, Knut
T1 - Sialyl-Tn Antigen-Imprinted Dual Fluorescent Core–Shell Nanoparticles for Ratiometric Sialyl-Tn Antigen Detection and Dual-Color Labeling of Cancer Cells
N2 - Sialyl-Tn (STn or sialyl-Thomsen-nouveau) is a carbohydrate antigen expressed by more than 80% of human carcinomas. We here report a strategy for ratiometric STn detection and dual-color cancer cell labeling, particularly, by molecularly imprinted polymers (MIPs). Imprinting was based on spectroscopic studies of a urea-containing green-fluorescent monomer 1 and STn-Thr-Na (sodium salt of Neu5Acα2-6GalNAcα-O-Thr). A few-nanometer-thin green-fluorescent polymer shell, in which STn-Thr-Na was imprinted with 1, other comonomers, and a cross-linker, was synthesized from the surface of red-emissive carbon nanodot (R-CND)-doped silica nanoparticles, resulting in dual fluorescent STn-MIPs. Dual-color labeling of cancer cells was achieved since both red and green emissions were detected in two separate channels of the microscope and an improved accuracy was obtained in comparison with single-signal MIPs. The flow cytometric cell analysis showed that the binding of STn-MIPs was significantly higher (p < 0.001) than that of non-imprinted polymer (NIP) control particles within the same cell line, allowing to distinguish populations. Based on the modularity of the luminescent core–fluorescent MIP shell architecture, the concept can be transferred in a straightforward manner to other target analytes.
KW - Cancer
KW - Core−shell particles
KW - Dual-color labeling glycan
KW - Molecular imprinting
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563106
DO - https://doi.org/10.1021/acsanm.2c03252
SP - 1
EP - 14
PB - ACS Publications
AN - OPUS4-56310
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Junge, Florian
A1 - Wittwer, Philipp
A1 - Sommerfeld, Thomas
A1 - Gehrenkemper, Lennart
A1 - Zoister, Christian
A1 - Nickl, Philip
A1 - Koch, Matthias
A1 - Meermann, Björn
A1 - Haag, Rainer
T1 - Adsorber Charge Dominates over Hydrophobic or Fluorophilic Functionalization in Influencing Adsorption of PFCA onto Polystyrene Resins
N2 - A systematic series of industrial-relevant polystyrene-based anion exchange resins that are functionalized with hydro- or fluorocarbon chains are compared regarding their adsorption behavior toward perfluorocarboxylic acids (PFCA) in respect to their charge, chain length, and type of chain. The results clearly show the dominance of electrostatic interactions in the adsorption process as uncharged adsorber materials showed no adsorption at all. In contrast, the charged adsorber materials showed in general a PFCA removal of 80% to 30% over the experiment depending on effluent fraction.
Unexpectedly, for perfluorobutanoic acid (PFBA) the highest removal rate is found with consistently >90%. Despite observing significant benefits in the adsorption of PFCA for fluoroalkylated adsorbers in comparison to their non-fluorinated counterparts, this effect of fluoroalkylation is comparatively small and can not be clearly attributed to fluorophilic interactions between the fluoroalkyl chains. These findings help clarifying that the introduction of fluorocarbon moieties in adsorber materials is not necessary in order to remove fluorocarbon molecules from the environment.
KW - PFAS
KW - Remediation
KW - Adsorption
KW - Fluorophilic interactions
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601883
DO - https://doi.org/10.1002/admi.202400199
SN - 2196-7350
SP - 1
EP - 10
PB - John Wiley & Sons
CY - Hoboken, New Jersey, USA
AN - OPUS4-60188
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kader, A.
A1 - Brangsch, J.
A1 - Kaufmann, Jan Ole
A1 - Zhao, J.
A1 - Mangarova, D. B.
A1 - Moeckel, J.
A1 - Adams, L. C.
A1 - Sack, I.
A1 - Taupitz, M.
A1 - Hamm, B.
A1 - Makowski, M. R.
T1 - Molecular MR Imaging of Prostate Cancer
N2 - This review summarizes recent developments regarding molecular imaging markers for magnetic resonance imaging (MRI) of prostate cancer (PCa). Currently, the clinical standard includes MR imaging using unspecific gadolinium-based contrast agents. Specific molecular probes for the diagnosis of PCa could improve the molecular characterization of the tumor in a non-invasive examination. Furthermore, molecular probes could enable targeted therapies to suppress tumor growth or reduce the tumor size.
KW - Prostate cancer
KW - Magnetic resonance imaging
KW - Molecular imaging
KW - Imaging
KW - Molecular marker
KW - Screening
KW - MRI
KW - Diagnosis
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519503
DO - https://doi.org/10.3390/biomedicines9010001
VL - 9
IS - 1
SP - 1
EP - 17
PB - MDPI
CY - Basel
AN - OPUS4-51950
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kader, A.
A1 - Brangsch, J.
A1 - Reimann, C.
A1 - Kaufmann, Jan Ole
A1 - Mangarova, D. B.
A1 - Moeckel, J.
A1 - Adams, L. C.
A1 - Zhao, J.
A1 - Saatz, Jessica
A1 - Traub, Heike
A1 - Buchholz, R.
A1 - Karst, U.
A1 - Hamm, B.
A1 - Makowski, M. R.
T1 - Visualization and Quantification of the Extracellular Matrix in Prostate Cancer Using an Elastin Specific Molecular Probe
N2 - One of the most commonly diagnosed cancers in men is prostate cancer (PCa). Understanding tumor progression can help diagnose and treat the disease at an early stage. Components of the extracellular matrix (ECM) play a key role in the development and progression of PCa. Elastin is an essential component of the ECM and constantly changes during tumor development. This article visualizes and quantifies elastin in magnetic resonance imaging (MRI) using a small molecule probe. Results were correlated with histological examinations. Using an elastin-specific molecular probe, we were able to make predictions about the cellular structure in relation to elastin and thus draw conclusions about the size of the tumor, with smaller tumors having a higher elastin content than larger tumors.
Human prostate cancer (PCa) is a type of malignancy and one of the most frequently diagnosed cancers in men. Elastin is an important component of the extracellular matrix and is involved in the structure and organization of prostate tissue. The present study examined prostate cancer in a xenograft mouse model using an elastin-specific molecular probe for magnetic resonance molecular imaging. Two different tumor sizes (500 mm3 and 1000 mm3) were compared and analyzed by MRI in vivo and histologically and analytically ex vivo. The T1-weighted sequence was used in a clinical 3-T scanner to calculate the relative contrast enhancement before and after probe administration. Our results show that the use of an elastin-specific probe enables better discrimination between tumors and surrounding healthy tissue. Furthermore, specific binding of the probe to elastin fibers was confirmed by histological examination and laser ablation–inductively coupled plasma–mass spectrometry (LA-ICP-MS). Smaller tumors showed significantly higher signal intensity (p > 0.001), which correlates with the higher proportion of elastin fibers in the histological evaluation than in larger tumors. A strong correlation was seen between relative enhancement (RE) and Elastica–van Gieson staining (R2 = 0.88). RE was related to inductively coupled plasma–mass spectrometry data for Gd and showed a correlation (R2 = 0.78). Thus, molecular MRI could become a novel quantitative tool for the early evaluation and detection of PCa.
KW - Magnetic resonance imaging
KW - MRI
KW - Molecular imaging
KW - Cancer
KW - LA-ICP-MS
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538410
DO - https://doi.org/10.3390/biology10111217
VL - 10
IS - 11
SP - 1
EP - 14
PB - MDPI
CY - Basel
AN - OPUS4-53841
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kader, A.
A1 - Kaufmann, Jan Ole
A1 - Mangarova, D. B.
A1 - Moeckel, J.
A1 - Adams, L. C.
A1 - Brangsch, J.
A1 - Heyl, J. L.
A1 - Zhao, J.
A1 - Verlemann, C.
A1 - Karst, U.
A1 - Collettini, F.
A1 - Auer, T. A.
A1 - Hamm, B.
A1 - Makowski, M. R.
T1 - Collagen-specific molecular magnetic resonance imaging of prostate cancer
N2 - Constant interactions between tumor cells and the extracellular matrix (ECM) influence the progression of prostate cancer (PCa). One of the key components of the ECM are collagen fibers, since they are responsible for the tissue stiffness, growth, adhesion, proliferation, migration, invasion/metastasis, cell signaling, and immune recruitment of tumor cells. To explore this molecular marker in the content of PCa, we investigated two different tumor volumes (500 mm3 and 1000 mm3) of a xenograft mouse model of PCa with molecular magnetic resonance imaging (MRI) using a collagen-specific probe. For in vivo MRI evaluation, T1-weighted sequences before and after probe administration were analyzed. No significant signal difference between the two tumor volumes could be found. However, we detected a significant difference between the signal intensity of the peripheral tumor area and the central area of the tumor, at both 500 mm3 (p < 0.01, n = 16) and at 1000 mm3 (p < 0.01, n = 16). The results of our histologic analyses confirmed the in vivo studies: There was no significant difference in the amount of collagen between the two tumor volumes (p > 0.05), but within the tumor, higher collagen expression was observed in the peripheral area compared with the central area of the tumor. Laser ablation with inductively coupled plasma mass spectrometry further confirmed these results. The 1000 mm3 tumors contained 2.8 +- 1.0% collagen and the 500 mm3 tumors contained 3.2 +- 1.2% (n = 16). There was a strong correlation between the in vivo MRI data and the ex vivo histological data (y = 0.068x + 1.1; R2 = 0.74) (n = 16). The results of elemental analysis by inductively coupled plasma mass spectrometry supported the MRI data (y = 3.82x + 0.56; R2 = 0.79; n = 7). MRI with the collagen-specific probe in PCa enables differentiation between different tumor areas. This may help to differentiate tumor from healthy tissue, potentially identifying tumor areas with a specific tumor biology.
KW - Molecular imaging
KW - Magnetic resonance imaging
KW - MRI
KW - Prostate cancer
KW - Collagen
KW - Laser ablation-inductively coupled plasma-mass spectroscopy
KW - EP-3533
KW - Peptide probe
KW - Gd-DOTA
KW - Contrast agent
KW - Tumor
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568449
DO - https://doi.org/10.3390/ijms24010711
SN - 1422-0067
SN - 1661-6596
VL - 24
IS - 1
SP - 1
EP - 13
PB - MDPI
CY - Basel
AN - OPUS4-56844
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kader, A.
A1 - Kaufmann, Jan Ole
A1 - Mangarova, D. B.
A1 - Moeckel, J.
A1 - Brangsch, J.
A1 - Adams, L. C.
A1 - Zhao, J.
A1 - Reimann, C.
A1 - Saatz, Jessica
A1 - Traub, Heike
A1 - Buchholz, R.
A1 - Karst, U.
A1 - Hamm, B.
A1 - Makowski, M. R.
T1 - Iron Oxide Nanoparticles for Visualization of Prostate Cancer in MRI
N2 - Prostate cancer (PCa) is one of the most common cancers in men. For detection and diagnosis of PCa, non-invasive methods, including magnetic resonance imaging (MRI), can reduce the risk potential of surgical intervention. To explore the molecular characteristics of the tumor, we investigated the applicability of ferumoxytol in PCa in a xenograft mouse model in two different tumor volumes, 500 mm3 and 1000 mm3. Macrophages play a key role in tumor progression, and they are able to internalize iron-oxide particles, such as ferumoxytol. When evaluating T2*-weighted sequences on MRI, a significant decrease of signal intensity between pre- and post-contrast images for each tumor volume (n = 14; p < 0.001) was measured. We, furthermore, observed a higher signal loss for a tumor volume of 500 mm3 than for 1000 mm3. These findings were confirmed by histological examinations and laser ablation inductively coupled plasma-mass spectrometry. The 500 mm3 tumors had 1.5% iron content (n = 14; sigma = 1.1), while the 1000 mm3 tumors contained only 0.4% iron (n = 14; sigma = 0.2). In vivo MRI data demonstrated a correlation with the ex vivo data (R2 = 0.75). The results of elemental analysis by inductively coupled plasma-mass spectrometry correlated strongly with the MRI data (R2 = 0.83) (n = 4). Due to its long retention time in the blood, biodegradability, and low toxicity to patients, ferumoxytol has great potential as a contrast agent for visualization PCa.
KW - Imaging
KW - Nanoparticle
KW - Cancer
KW - Iron oxide
KW - ICP-MS
KW - Magnetic resonance imaging
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550075
DO - https://doi.org/10.3390/cancers14122909
VL - 14
IS - 12
SP - 1
EP - 13
PB - MDPI
CY - Basel, Switzerland
AN - OPUS4-55007
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kader, A.
A1 - Snellings, J.
A1 - Adams, L. C.
A1 - Gottheil, P.
A1 - Mangarova, D. B.
A1 - Heyl, J. L.
A1 - Kaufmann, Jan Ole
A1 - Moeckel, J.
A1 - Brangsch, J.
A1 - Auer, T. A.
A1 - Collettini, F.
A1 - Sauer, F.
A1 - Hamm, B.
A1 - Käs, J.
A1 - Sack, I.
A1 - Makowski, M. R.
A1 - Braun, J.
T1 - Sensitivity of magnetic resonance elastography to extracellular matrix and cell motility in human prostate cancer cell line-derived xenograft models
N2 - Prostate cancer (PCa) is a significant health problem in the male population of the Western world. Magnetic resonance elastography (MRE), an emerging medical imaging technique sensitive to mechanical properties of biological tissues, detects PCa based on abnormally high stiffness and viscosity values. Yet, the origin of these changes in tissue properties and how they correlate with histopathological markers and tumor aggressiveness are largely unknown, hindering the use of tumor biomechanical properties for establishing a noninvasive PCa staging system.
To infer the contributions of extracellular matrix (ECM) components and cell motility, we investigated fresh tissue specimens from two PCa xenograft mouse models, PC3 and LNCaP, using magnetic resonance elastography (MRE), diffusion-weighted imaging (DWI), quantitative histology, and nuclear shape analysis. Increased tumor stiffness and impaired water diffusion were observed to be associated with collagen and elastin accumulation and decreased cell motility. Overall, LNCaP, while more representative of clinical PCa than PC3, accumulated fewer ECM components, induced less restriction of water diffusion, and exhibited increased cell motility, resulting in overall softer and less viscous properties. Taken together, our results suggest that prostate tumor stiffness increases with ECM accumulation and cell adhesion - characteristics that influence critical biological processes of cancer development.
MRE paired with DWI provides a powerful set of imaging markers that can potentially predict prostate tumor development from benign masses to aggressive malignancies in patients. Statement of significance: Xenograft models of human prostate tumor cell lines, allowing correlation of microstructure-sensitive biophysical imaging parameters with quantitative histological methods, can be investigated to identify hallmarks of cancer.
KW - Magnetic resonance elastography
KW - Quantitative histology
KW - Prostate cancer
KW - Stiffness
KW - Fluidity
KW - Apparent diffusion coefficient
KW - Collagen
KW - Elastin
KW - Nuclear shape
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618361
DO - https://doi.org/10.1016/j.bioadv.2024.213884
SN - 2772-9508
VL - 161
SP - 1
EP - 12
PB - Elsevier
CY - Amsterdam
AN - OPUS4-61836
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kage, Daniel
A1 - Hoffmann, Katrin
A1 - Borcherding, H.
A1 - Schedler, U.
A1 - Resch-Genger, Ute
T1 - Lifetime encoding in flow cytometry for bead‑based sensing of biomolecular interaction
N2 - To demonstrate the potential of time-resolved flow cytometry (FCM) for bioanalysis, clinical diagnostics, and optically encoded bead-based assays, we performed a proof-of-principle study to detect biomolecular interactions utilizing fluorescence lifetime (LT)-encoded micron-sized polymer beads bearing target-specific bioligands and a recently developed prototype lifetime flow cytometer (LT-FCM setup). This instrument is equipped with a single excitation light source and different fluorescence detectors, one operated in the photon-counting mode for time-resolved measurements of fluorescence decays and three detectors for conventional intensity measurements in different spectral windows. First, discrimination of bead-bound biomolecules was demonstrated in the time domain exemplarily for two targets, Streptavidin (SAv) and the tumor marker human chorionic gonadotropin (HCG). In a second step, the determination of biomolecule concentration levels was addressed representatively for the inflammation-related biomarker tumor necrosis factor (TNF-α) utilizing fluorescence intensity measurements in a second channel of the LT-FCM instrument. Our results underline the applicability of LT-FCM in the time domain for measurements of biomolecular interactions in suspension assays. In the future, the combination of spectral and LT encoding and multiplexing and the expansion of the time scale from the lower nanosecond range to the longer nanosecond and the microsecond region is expected to provide many distinguishable codes. This enables an increasing degree of multiplexing which could be attractive for high throughput screening applications.
KW - Fluorescence
KW - Sensor
KW - Assay
KW - Protein
KW - Multiplexing
KW - Flow cytometry
KW - Barcoding
KW - Lifetime
KW - Dye
KW - Bead
KW - Bead-based assay
KW - Method
KW - Quantification
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516007
DO - https://doi.org/10.1038/s41598-020-76150-x
VL - 10
IS - 1
SP - 19477
PB - Nature
AN - OPUS4-51600
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kage, Daniel
A1 - Hoffmann, Katrin
A1 - Nifontova, G.
A1 - Krivenkov, V.
A1 - Sukhanova, A.
A1 - Nabiev, I.
A1 - Resch-Genger, Ute
T1 - Tempo-spectral multiplexing in flow cytometry with lifetime detection using QD-encoded polymer beads
N2 - Semiconductor quantum dots (QDs) embedded into polymer microbeads are known to be very attractive emitters for spectral multiplexing and colour encoding. Their luminescence lifetimes or decay kinetics have been, however, rarely exploited as encoding parameter, although they cover time ranges which are not easily accessible with other luminophores. We demonstrate here the potential of QDs made from II/VI semiconductors with luminescence lifetimes of several 10 ns to expand the lifetime range of organic encoding luminophores in multiplexing applications using time-resolved flow cytometry (LT-FCM). For this purpose, two different types of QD-loaded beads were prepared and characterized by photoluminescence measurements on the ensemble level and by single-particle confocal laser scanning microscopy. Subsequently, these lifetime-encoded microbeads were combined with dye-encoded microparticles in systematic studies to demonstrate the potential of these QDs to increase the number of lifetime codes for lifetime multiplexing and combined multiplexing in the time and colour domain (tempo-spectral multiplexing). These studies were done with a recently developed novel luminescence lifetime flow cytometer (LT-FCM setup) operating in the time-domain, that presents an alternative to reports on phase-sensitive lifetime detection in flow cytometry.
KW - Fluorescence life time
KW - Flow cytometry
KW - Lifetime-encoded beads
KW - Quantum dots
KW - Multiplexing
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503316
DO - https://doi.org/10.1038/s41598-019-56938-2
VL - 10
IS - 1
SP - Article number: 653
PB - nature.com
AN - OPUS4-50331
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kalbe, Ute
A1 - Piechotta, Christian
A1 - Bandow, Nicole
T1 - Comparing PFAS analysis in batch leaching and column leaching tests
N2 - Laboratory leaching tests are tools to assess the mobility of environmental contaminants released from granular materials. Comparative leaching tests were performed using four PFAS-contaminated soils whose concentration patterns of 10 selected perfluoroalkyl and polyfluoroalkyl substances (PFAS) differed due to the two types of contamination sources. This study aimed to evaluate the equivalence of two usual laboratory-scale leaching test procedures, batch and column percolation tests, at liquid-to-solid ratios (L/S) of 2 l/kg, which is the current practice within the German assessment framework, and 10 l/kg (relevant for some EU regulations such as the landfill directive). The differences between the replicates of leaching tests investigating PFAS were smaller for column percolation tests than for batch tests, probably mainly due to the greater sample size and the better representativeness of the sample portion analyzed. It was observed that batch tests overestimate the release of shorter-chain PFAS, whereby the effect was greater with carboxylic than with sulfonic acids. Currently, the limits of detection of analyses given by the DIN standard with regard to PFCA and PFSA in soils are partly not sufficient to detect very low contents, whereas the detection of selected PFCA and PFSA in eluates is more sensitive, in accordance with the available standards. This results in limitations when calculating mass balances.
KW - PFAS
KW - Leaching
KW - Column percolation test
KW - Batch test
KW - Soil
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618187
DO - https://doi.org/10.1007/s11356-024-35510-0
SN - 1614-7499
VL - 31
IS - 57
SP - 65233
EP - 65251
PB - Springer Science and Business Media LLC
AN - OPUS4-61818
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kalmbach, J.
A1 - Wang, Cui
A1 - You, Yi
A1 - Förster, C.
A1 - Schubert, H.
A1 - Heinze, K.
A1 - Resch-Genger, Ute
A1 - Seitz, M.
T1 - Near-IR to near-IR upconversion luminescence in molecular chromium ytterbium salts
N2 - Upconversion photoluminescence in hetero-oligonuclear metal complex architectures featuring organic ligands is an interesting but still rarely observed phenomenon, despite its great potential from a basic research and application perspective. In this context, a new photonic material consisting of molecular chromium(III) and ytterbium(III) complex Ions was developed that exhibits excitation-power density-dependent cooperative sensitization of the chromium-centered 2E/2T1 phosphorescence at approximately 775 nm after excitation of the ytterbium band 2F7/2!2F5/2 at approximately 980 nm in the solid state at ambient temperature. The upconversion process is insensitive to atmospheric oxygen and can be observed in the presence of water molecules in the crystal lattice.
KW - Upconversion
KW - Lanthanide
KW - Photoluminescence
KW - Quantum yield
KW - Photophysics
KW - Lifetime
KW - Sensor
KW - NIR
KW - Cr(III)
KW - Yb(III) complex
KW - Crystal
KW - Triplet-triplet annihilation
KW - Sensitization
KW - Light harvesting
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512619
DO - https://doi.org/10.1002/anie.202007200
SN - 1433-7851
SN - 1521-3773
VL - 59
IS - 42
SP - 18804
EP - 18808
PB - Wiley
CY - Weinheim
AN - OPUS4-51261
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kalot, G.
A1 - Godard, A.
A1 - Busser, B.
A1 - Pliquett, J.
A1 - Broekgaarden, M.
A1 - Motto-Ros, V.
A1 - Wegner, Karl David
A1 - Resch-Genger, Ute
A1 - Köster, U.
A1 - Denat, F.
A1 - Coll, J.-L.
A1 - Bodio, E.
A1 - Goze, C.
A1 - Sancey, L.
T1 - Aza-BODIPY: A New Vector for Enhanced Theranostic Boron Neutron Capture Therapy Applications
N2 - Boron neutron capture therapy (BNCT) is a radiotherapeutic modality based on the nuclear capture of slow neutrons by stable 10B atoms followed by charged particle Emission that inducing extensive damage on a very localized level (<10 um). To be effcient, a suffcient amount of 10B should accumulate in the tumor area while being almost cleared from the normal surroundings. A water-soluble aza-boron-dipyrromethene dyes (BODIPY) fluorophore was reported to strongly accumulate in the tumor area with high and BNCT compatible Tumor/Healthy Tissue ratios.
The clinically used 10B-BSH (sodium borocaptate) was coupled to the water-soluble aza-BODIPY platform for enhanced 10B-BSH tumor vectorization. We demonstrated a strong uptake of the compound in tumor cells and determined its biodistribution in mice-bearing tumors. A model of chorioallantoic membrane-bearing glioblastoma xenograft was developed to evidence the BNCT potential of such compound, by subjecting it to slow neutrons. We demonstrated the Tumor accumulation of the compound in real-time using optical imaging and ex vivo using elemental imaging based on laser-induced breakdown spectroscopy. The tumor growth was significantly reduced as compared to BNCT with 10B-BSH. Altogether, the fluorescent aza-BODIPY/10B-BSH compound is able to vectorize and image the 10B-BSH in the tumor area, increasing its theranostic potential for effcient approach of BNCT.
KW - Aza-BODIPY
KW - SWIR
KW - NIR-I
KW - Theranostic
KW - Boron compound
KW - Optical imaging
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512280
DO - https://doi.org/10.3390/cells9091953
VL - 9
IS - 9
SP - 1953
PB - MDPI
AN - OPUS4-51228
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kamdem Tamo, Arnaud
A1 - Doench, Ingo
A1 - Deffo, Gullit
A1 - Jiokeng, Sherman Lesly Zambou
A1 - Doungmo, Giscard
A1 - Fotsop, Cyrille Ghislain
A1 - Temgoua, Ranil Clement Tonleu
A1 - Montembault, Alexandra
A1 - Serghe, Anatoli
A1 - Njanja, Evangeline
A1 - Tonle, Ignas Kenfack
A1 - Osorio-Madrazo, Anayancy
T1 - Lignocellulosic biomass and its main structural polymers as sustainable materials for (bio)sensing applications
N2 - (Bio)sensors are integral to various aspects of daily life, contributing to safety, monitoring, and awareness. In modern sensor devices, polymers play an important role, with increasing interest in bio-based materials. Biopolymers, unlike their synthetic counterparts, are abundant in nature and exhibit interesting functional properties that make them highly suitable as biomaterials for sensor technologies. Enhancing sensor performance to achieve a rapid response to stimuli is a key objective in sensor development. Lignocellulosic biomass (LCB) from plants holds promise in meeting such requirements due to its high surface area, tunable surface characteristics (including diverse pore sizes and morphologies), flexibility, printability, low density, and favorable physicochemical and thermal properties. Growing research in recent decades has focused on lignocellulosic composite materials due to their functional and environmentally friendly attributes. This review focuses on the valorization of lignocellulosic biomass and its three main biopolymer constituents (cellulose, hemicellulose, and lignin) for the development of electrochemical (bio)sensors. It also explores the macromolecular structure, sources, and inherent properties of LCB, with emphasis on the three main biopolymers and their applications in sensor technologies. Recent advances in the use of LCB and its structural biopolymers as materials for (bio)sensing applications are described and reviewed. The challenges associated with using these biomaterials in electroanalytical applications are also discussed, along with the exploration of their future potential for developing high-performance sensing technologies.
KW - Chemical safety
KW - Material safety
KW - Quality ensurance
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637230
DO - https://doi.org/10.1039/d5ta02900g
SN - 2050-7496
SP - 1
EP - 69
PB - The Royal Society of Chemistry
AN - OPUS4-63723
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kang, Y.
A1 - Nack, L. M.
A1 - Liu, Y.
A1 - Qi, B.
A1 - Huang, Y.
A1 - Liu, Z.
A1 - Chakraborty, I.
A1 - Schulz, F.
A1 - Ahmed, A. A. A.
A1 - Poveda, M. C.
A1 - Hafizi, F.
A1 - Roy, S.
A1 - Mutas, M.
A1 - Holzapfel, M.
A1 - Sanchez-Cano, C.
A1 - Wegner, Karl David
A1 - Feliu, N.
A1 - Parak, W. J.
T1 - Quantitative considerations about the size dependence of cellular entry and excretion of colloidal nanoparticles for different cell types
N2 - Most studies about the interaction of nanoparticles (NPs) with cells have focused on how the physicochemical properties of NPs will influence their uptake by cells. However, much less is known about their potential excretion from cells. However, to control and manipulate the number of NPs in a cell, both cellular uptake and excretion must be studied quantitatively. Monitoring the intracellular and extracellular amount of NPs over time (after residual noninternalized NPs have been removed) enables one to disentangle the influences of cell proliferation and exocytosis, the major pathways for the reduction of NPs per cell. Proliferation depends on the type of cells, while exocytosis depends in addition on properties of the NPs, such as their size. Examples are given herein on the role of these two different processes for different cells and NPs.
KW - Cell proliferation
KW - Exocytosis
KW - Gold nanoparticles
KW - Quantum dots
KW - Fluorescence
KW - Uptake studies
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543476
DO - https://doi.org/10.1007/s40828-021-00159-6
SN - 2199-3793
VL - 8
IS - 1
SP - 1
EP - 8
PB - Springer
CY - Berlin
AN - OPUS4-54347
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kaufmann, Jan Ole
A1 - Brangsch, J.
A1 - Kader, A.
A1 - Saatz, Jessica
A1 - Mangarova, D. B.
A1 - Zacharias, M.
A1 - Kempf, W. E.
A1 - Schwaar, T.
A1 - Ponader, Marco
A1 - Adams, L. C.
A1 - Möckel, J.
A1 - Botnar, R. M.
A1 - Taupitz, M.
A1 - Mägdefessel, L.
A1 - Traub, Heike
A1 - Hamm, B.
A1 - Weller, Michael G.
A1 - Makowski, M. R.
T1 - ADAMTS4-specific MR-probe to assess aortic aneurysms in vivo using synthetic peptide libraries
N2 - The incidence of abdominal aortic aneurysms (AAAs) has substantially increased during the last 20 years and their rupture remains the third most common cause of sudden death in the cardiovascular field after myocardial infarction and stroke. The only established clinical parameter to assess AAAs is based on the aneurysm size. Novel biomarkers are needed to improve the assessment of the risk of rupture. ADAMTS4 (A Disintegrin And Metalloproteinase with ThromboSpondin motifs 4) is a strongly upregulated proteoglycan cleaving enzyme in the unstable course of AAAs. In the screening of a one-bead-one-compound library against ADAMTS4, a low-molecular-weight cyclic peptide is discovered with favorable properties for in vivo molecular magnetic resonance imaging applications. After identification and characterization, it’s potential is evaluated in an AAA mouse model. The ADAMTS4-specific probe enables the in vivo imaging-based prediction of aneurysm expansion and rupture.
KW - Peptide
KW - Peptide library
KW - OBOC library
KW - Combinatorial chemistry
KW - Peptide aptamers
KW - Binding molecule
KW - Affinity
KW - Synthetic peptides
KW - Contrast agent
KW - Magnetic resonance imaging
KW - One-bead-one-compound library
KW - On-chip screening
KW - Lab-on-a-chip
KW - MALDI-TOF MS
KW - SPR
KW - Surface plasmon resonance
KW - Alanine scan
KW - Fluorescence label
KW - MST
KW - Docking
KW - Chelate
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560930
DO - https://doi.org/10.1038/s41467-022-30464-8
N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M.
VL - 13
IS - 1
SP - 1
EP - 18
PB - Springer Nature Limited
CY - Heidelberg
AN - OPUS4-56093
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kazlagić, Anera
A1 - Rosner, M.
A1 - Cipriani, A.
A1 - Frick, D. A.
A1 - Glodny, J.
A1 - Hoffmann, E. J.
A1 - Hora, J. M.
A1 - Irrgeher, J.
A1 - Lugli, F.
A1 - Magna, T.
A1 - Meisel, T. C.
A1 - Meixner, A.
A1 - Possolo, A.
A1 - Pramann, A.
A1 - Pribil, M. J.
A1 - Prohaska, T.
A1 - Retzmann, Anika
A1 - Rienitz, O.
A1 - Rutherford, D.
A1 - Paula-Santos, G. M.
A1 - Tatzel, M.
A1 - Widhalm, S.
A1 - Willbold, M.
A1 - Zuliani, T.
A1 - Vogl, Jochen
T1 - Characterisation of conventional 87Sr/86Sr isotope ratios in cement, limestone and slate reference materials based on an interlaboratory comparison study
N2 - An interlaboratory comparison (ILC)was organised to characterise 87Sr/86Sr isotope ratios in geological and industrial reference materials by applying the so-called conventional method for determining 87Sr/86Sr isotope ratios. Four cements (VDZ 100a,VDZ 200a, VDZ 300a, IAG OPC-1), one limestone (IAG CGL ML-3) and one slate (IAG OU-6) reference materials were selected, covering a wide range of naturally occurring Sr isotopic signatures. Thirteen laboratories received aliquots of these six reference materials together with a detailed technical protocol. The consensus values for the six reference materials and their associated measurement uncertainties were obtained by applying a Gaussian, linear mixed effects model fitted to all the measurement results. By combining the consensus values and their uncertainties with an uncertainty contribution for potential heterogeneity, reference values ranging from 0.708134 mol mol-1 to 0.729778 mol mol-1 were obtained with relative expanded uncertainties of ≤ 0.007 %. This study represents an ILC on conventional 87Sr/86Sr isotope ratios, within which metrological principles were considered and the compatibility of measurement results obtained by MC-ICP-MS and by MC-TIMS is demonstrated. The materials characterised in this study can be used as reference materials for validation and quality control purposes and to estimate measurement uncertainties in conventional 87Sr/86Sr isotope ratio measurement.
KW - Sr isotope analysis
KW - Isotope ratios
KW - Cement
KW - Geological material
KW - MC-TIMS
KW - MC-ICP-MS
KW - Interlaboratory comparison
KW - Measurement uncertainty
KW - Cconventional method
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579836
DO - https://doi.org/10.1111/ggr.12517
SN - 1639-4488
VL - 47
IS - 4
SP - 821
EP - 840
PB - Wiley online library
AN - OPUS4-57983
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kazlagić, Anera
A1 - Russo, Francesco
A1 - Vogl, Jochen
A1 - Sturm, Patrick
A1 - Stephan, D.
A1 - Gluth, Gregor
ED - Resch-Genger, Ute
ED - Koch, Matthias
ED - Meermann, Björn
ED - Weller, Michael G.
T1 - Development of a sample preparation procedure for Sr isotope analysis of Portland cements
N2 - The 87Sr/86Sr isotope ratio can, in principle, be used for provenancing of cement. However, while commercial cements consist of multiple components, no detailed investigation into their individual 87Sr/86Sr isotope ratios or their influence on the integral 87Sr/86Sr isotope ratio of the resulting cement was conducted previously. Therefore, the present study aimed at determining and comparing the conventional 87Sr/86Sr isotope ratios of a diverse set of Portland cements and their corresponding Portland clinkers, the major component of these cements. Two approaches to remove the additives from the cements, i.e. to measure the conventional 87Sr/86Sr isotopic fingerprint of the clinker only, were tested, namely, treatment with a potassium hydroxide/sucrose solution and sieving on a 11-µm sieve. Dissolution in concentrated hydrochloric acid/nitric acid and in diluted nitric acid was employed to determine the 87Sr/86Sr isotope ratios of the cements and the individual clinkers. The aim was to find the most appropriate sample preparation procedure for cement provenancing, and the selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated cements with those of the corresponding clinkers. None of the methods to separate the clinkers from the cements proved to be satisfactory. However, it was found that the 87Sr/86Sr isotope ratios of clinker and cement generally corresponded, meaning that the latter can be used as a proxy for the clinker 87Sr/86Sr isotope ratio. Finally, the concentrated hydrochloric acid/nitric acid dissolution method was found to be the most suitable sample preparation method for the cements; it is thus recommended for 87Sr/86Sr isotope analyses for cement provenancing.
KW - Cement
KW - Provenancing
KW - Sr isotopes
KW - Portland clinker
KW - Dissolution
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542239
DO - https://doi.org/10.1007/s00216-021-03821-7
SN - 1618-2642
SN - 1618-2650
VL - 414
IS - 15 (Topical collection: Analytical methods and applications in the materials and life sciences)
SP - 4379
EP - 4389
PB - Springer
CY - Berlin
AN - OPUS4-54223
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kazlagić, Anera
A1 - Vogl, Jochen
A1 - Gluth, Gregor
A1 - Stephan, D.
T1 - Provenancing of cement using elemental analyses and isotope techniques – The state-of-the-art and future perspectives
N2 - With the aim of identifying the origin and the manufacturer of a cement, a reliable procedure that provides unambiguous results is needed. Such procedure could resolve practical issues in damage research, liability issues and forensic investigations. A substantial number of attempts for fingerprinting of building materials, including cement, has already been carried out during the last decades. Most of them were based on concentration analysis of the main elements/components. This review provides an overview of provenance studies of cement and the main approaches commonly used. Provenance studies of cement via isotope techniques are also presented and discussed as representatives of the state-of-the-art in the field. Due to the characteristic properties and the occurrence of carefully selected isotope ratios, unique fingerprints of different kinds of materials can be provided by these methods. This property has largely been explored in various scientific fields such as geo- and cosmochemistry, food forensics, archaeology, geochronology, biomedical studies, and climate change processes. However, the potential of isotope techniques in cement and concrete research for provenance studies has barely been investigated.
Therefore, the review outlines a suitable approach using isotope ratios, which could lead to reliable provenancing of cementitious materials in the future.
KW - Cement
KW - Sr isotopes
KW - Provenance
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533762
DO - https://doi.org/10.1039/d1ja00144b
VL - 36
IS - 10
SP - 2030
EP - 2042
PB - The Royal Society of Chemistry
CY - Cambridge, UK
AN - OPUS4-53376
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Keller, S.
A1 - Borde, T.
A1 - Brangsch, J.
A1 - Reimann, C.
A1 - Kader, A.
A1 - Schulze, D.
A1 - Buchholz, R.
A1 - Kaufmann, Jan Ole
A1 - Karst, U.
A1 - Schellenberger, E.
A1 - Hamm, B.
A1 - Makowski, M. R.
T1 - Assessment of the hepatic tumor extracellular matrix using elastin‑specific molecular magnetic resonance imaging in an experimental rabbit cancer model
N2 - To investigate the imaging performance of an elastin-specific molecular magnetic resonance imaging (MRI) probe with respect to the extracellular matrix (ECM) in an experimental hepatic cancer model. Twelve rabbits with hepatic VX2 tumors were examined using 3 T MRI 14, 21, and 28 days after tumor implantation for two subsequent days (gadobutrol, day 1; elastin-specific probe, day 2). The relative enhancement (RE) of segmented tumor regions (central and margin) and the peritumoral matrix was calculated using pre-contrast and delayed-phase T1w sequences. MRI measurements were correlated to histopathology and element-specific and spatially resolved mass spectrometry (MS). Mixed-model analysis was performed to assess the performance of the elastin-specific probe. In comparison to gadobutrol, the elastin probe showed significantly stronger RE, which was pronounced in the tumor margin (day 14–28: P ≤ 0.007). In addition, the elastin probe was superior in discriminating between tumor regions (χ2(4) = 65.87; P < 0.001). MRI-based measurements of the elastin probe significantly correlated with the ex vivo elastinstain (R = .84; P <0 .001) and absolute gadolinium concentrations (ICP-MS: R = .73, P <0 .01). LA-ICP-MS imaging confirmed the colocalization of the elastin-specific probe with elastic fibers. Elastin-specific molecular MRI is superior to non-specific gadolinium-based contrast agents in imaging the ECM of hepatic tumors and the peritumoral tissue.
KW - Elastin-specific molecular agent
KW - Extracellular matrix
KW - Hepatocellular carcinoma
KW - Inductively coupled plasma mass spectroscopy
KW - Laser ablation-inductively coupled plasma-mass spectrometry
KW - Magnetic resonance imaging
KW - MR imaging
KW - ESMA
KW - Gadolinium
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517360
DO - https://doi.org/10.1038/s41598-020-77624-8
VL - 10
IS - 1
SP - 20785
PB - Nature
AN - OPUS4-51736
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kern, Simon
A1 - Liehr, Sascha
A1 - Wander, Lukas
A1 - Bornemann-Pfeiffer, Martin
A1 - Müller, S.
A1 - Maiwald, Michael
A1 - Kowarik, Stefan
T1 - Artificial neural networks for quantitative online NMR spectroscopy
N2 - Industry 4.0 is all about interconnectivity, sensor-enhanced process control, and data-driven systems. Process analytical technology (PAT) such as online nuclear magnetic resonance (NMR) spectroscopy is gaining in importance, as it increasingly contributes to automation and digitalization in production. In many cases up to now, however, a classical evaluation of process data and their transformation into knowledge is not possible or not economical due to the insufficiently large datasets available. When developing an automated method applicable in process control, sometimes only the basic data of a limited number of batch tests from typical product and process development campaigns are available. However, these datasets are not large enough for training machine-supported procedures. In this work, to overcome this limitation, a new procedure was developed, which allows physically motivated multiplication of the available reference data in order to obtain a sufficiently large dataset for training machine learning algorithms. The underlying example chemical synthesis was measured and analyzed with both application-relevant low-field NMR and high-field NMR spectroscopy as reference method. Artificial neural networks (ANNs) have the potential to infer valuable process information already from relatively limited input data. However, in order to predict the concentration at complex conditions (many reactants and wide concentration ranges), larger ANNs and, therefore, a larger Training dataset are required. We demonstrate that a moderately complex problem with four reactants can be addressed using ANNs in combination with the presented PAT method (low-field NMR) and with the proposed approach to generate meaningful training data.
KW - Online NMR spectroscopy
KW - Real-time process monitoring
KW - Artificial neural networks
KW - Automation
KW - Process industry
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507508
DO - https://doi.org/10.1007/s00216-020-02687-5
SN - 1618-2642
VL - 412
IS - 18
SP - 4447
EP - 4459
PB - Springer
CY - Berlin
AN - OPUS4-50750
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kimani, Martha Wamaitha
A1 - Beyer, S.
A1 - El-Schich, Z.
A1 - Gawlitza, Kornelia
A1 - Rurack, Knut
A1 - Gjörloff-Wingren, A.
T1 - Imprinted Particles for Direct Fluorescence Detection of Sialic Acid in Polar Media and on Cancer Cells with Enhanced Control of Nonspecific Binding
N2 - Glycoproteins are abundant on the cell surface of mammals, providing structural support, modulating cell Membrane properties, and acting as signaling agents. Variation of glycosylation patterns has been found to indicate various disease states, including cell malignancy. Sialic acid (SA) is present as a terminating group on cell-surface glycans, and its overexpression has been linked to several types of cancer. Detection of SA on the cell surface is therefore critical for detection of cancer in its early stages. In this work, a fluorescent molecularly imprinted polymer layer targeting SA was synthesized on the surface of silica-coated polystyrene (PS) particles. Compared to previous works, a PS core supplies a lighter, lower-density support for improved suspension stability and scattering properties. Moreover, their smaller size provides a higher surface-area-to-volume ratio for binding. The incorporation of a fluorescent monomer in the MIP shell allowed for simple and rapid determination of binding specificity in polar media due to a deprotonation−reprotonation interaction mechanism between the fluorescent monomer and SA, which led to spectral changes.
Upon titration of the MIP particles with SA in suspension, an increase in fluorescence emission of the particles was observed, with the MIP particles binding SA more selectively compared to the nonimprinted polymer (NIP) control particles. In cell staining experiments performed by flow cytometry, the binding behavior of the MIP particles compared favorably with that of SA-binding lectins. NIPs prepared with a “dummy” template served as a better negative control in cell binding assays due to the favorable inward orientation of template-binding functional groups in the polymer shell, which reduced nonspecific binding. The results show that fluorescent MIPs targeting SA are a promising tool for in vitro fluorescence staining of cancerous cells and for future diagnosis of cancer at early stages.
KW - Flow cytometry
KW - Sialic acid
KW - Fluorescence
KW - Molecularly imprinted polymers
KW - Cancer cells
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525216
DO - https://doi.org/10.1021/acsapm.0c01353
VL - 3
IS - 5
SP - 2363
EP - 2373
PB - American Chemical Society
AN - OPUS4-52521
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kimani, Martha Wamaitha
A1 - Kislenko, Evgeniia
A1 - Gawlitza, Kornelia
A1 - Rurack, Knut
T1 - Fluorescent molecularly imprinted polymer particles for glyphosate detection using phase transfer agents
N2 - In this work, molecular imprinting was combined with direct fluorescence detection of the pesticide Glyphosate (GPS). Firstly, the solubility of highly polar GPS in organic solvents was improved by using lipophilic tetrabutylammonium (TBA+) and tetrahexylammonium (THA+) counterions. Secondly, to achieve fluorescence detection, a fluorescent crosslinker containing urea-binding motifs was used as a probe for GPS-TBA and GPS-THA salts in chloroform, generating stable complexes through hydrogen bond formation. The GPS/fluorescent dye complexes were imprinted into 2–3 nm fluorescent molecularly imprinted polymer (MIP) shells on the surface of sub-micron silica particles using chloroform as porogen. Thus, the MIP binding behavior could be easily evaluated by fluorescence titrations in suspension to monitor the spectral changes upon addition of the GPS analytes. While MIPs prepared with GPS-TBA and GPS-THA both displayed satisfactory imprinting following titration with the corresponding analytes in chloroform, GPS-THA MIPs displayed better selectivity against competing molecules. Moreover, the THA+ counterion was found to be a more powerful phase transfer agent than TBA+ in a biphasic assay, enabling the direct fluorescence detection and quantification of GPS in water. A limit of detection of 1.45 μM and a linear range of 5–55 μM were obtained, which match well with WHO guidelines for the acceptable daily intake of GPS in water (5.32 μM).
KW - Glyphosate
KW - Molecular imprinting
KW - Core-shell particles
KW - Fluorescent sensors
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555281
DO - https://doi.org/10.1038/s41598-022-16825-9
SN - 2045-2322
VL - 12
IS - 1
SP - 1
EP - 15
PB - Macmillan Publishers Limited
CY - London
AN - OPUS4-55528
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kimani, Martha Wamaitha
A1 - Pérez-Padilla, Victor
A1 - Valderrey, Virginia
A1 - Gawlitza, Kornelia
A1 - Rurack, Knut
T1 - Red-Emitting Polymerizable Guanidinium Dyes as Fluorescent Probes in Molecularly Imprinted Polymers for Glyphosate Detection
N2 - The development of methodologies to sense glyphosate has gained momentum due to its toxicological and ecotoxicological effects. In this work, a red-emitting and polymerizable guanidinium benzoxadiazole probe was developed for the fluorescence detection of glyphosate. The interaction of the fluorescent probe and the tetrabutylammonium salt of glyphosate was studied via UV/vis absorption and fluorescence spectroscopy in chloroform and acetonitrile. The selective recognition of glyphosate was achieved by preparing molecularly imprinted polymers, able to discriminate against other common herbicides such as 2,4-dichlorophenoxyacetic acid (2,4-D) and 3,6-dichloro-2-methoxybenzoic acid (dicamba), as thin layers on submicron silica particles. The limits of detection of 4.8 µM and 0.6 µM were obtained for the sensing of glyphosate in chloroform and acetonitrile, respectively. The reported system shows promise for future application in the sensing of glyphosate through further optimization of the dye and the implementation of a biphasic assay with water/organic solvent mixtures for sensing in aqueous environmental samples.
KW - Glyphosate
KW - Guanidinium receptors
KW - Fluorescent probes
KW - Molecularly imprinted polymers
KW - Core-shell particles
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544441
DO - https://doi.org/10.3390/chemosensors10030099
SN - 2227-9040
VL - 10
IS - 3
SP - 1
EP - 20
PB - MDPI
CY - Basel
AN - OPUS4-54444
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kirilina, E.
A1 - Helbling, S.
A1 - Morawski, M.
A1 - Pine, K.
A1 - Reimann, K.
A1 - Jankuhn, S.
A1 - Dinse, J.
A1 - Deistung, A.
A1 - Reichenbach, J. R.
A1 - Trampel, R.
A1 - Geyer, S.
A1 - Müller, Larissa
A1 - Jakubowski, Norbert
A1 - Arendt, T.
A1 - Bazin, P.-L.
A1 - Weiskopf, N.
T1 - Superficial white matter imaging: Contrast mechanisms and whole-brain in vivo mapping
N2 - Superficial white matter (SWM) contains the most cortico-cortical white matter connections in the human brain encompassing the short U-shaped association fibers. Despite its importance for brain connectivity, very little is known about SWM in humans, mainly due to the lack of noninvasive imaging methods. Here, we lay the groundwork for systematic in vivo SWM mapping using ultrahigh resolution 7 T magnetic resonance imaging. Using biophysical modeling informed by quantitative ion beam microscopy on postmortem brain tissue, we demonstrate that MR contrast in SWM is driven by iron and can be linked to the microscopic iron distribution. Higher SWM iron concentrations were observed in U-fiber–rich frontal, temporal, and parietal areas, potentially reflecting high fiber density or late myelination in these areas. Our SWM mapping approach provides the foundation for systematic studies of interindividual differences, plasticity, and pathologies of this crucial structure for cortico-cortical connectivity in humans.
KW - Magnetic resonance imaging
KW - Laser ablation
KW - ICP-MS
KW - Brain
KW - Imaging
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514430
DO - https://doi.org/10.1126/sciadv.aaz9281
SN - 2375-2548
VL - 6
IS - 41
SP - eaaz9281
PB - American Association for the Advancement of Science (Science/AAAS)
CY - Washington, DC, USA
AN - OPUS4-51443
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kislenko, Evgeniia
A1 - Incel, A.
A1 - Gawlitza, Kornelia
A1 - Sellergren, B.
A1 - Rurack, Knut
T1 - Towards molecularly imprinted polymers that respond to and capture phosphorylated tyrosine epitopes using fluorescent bis-urea and bis-imidazolium receptors
N2 - Early detection of cancer is essential for successful treatment and improvement in patient prognosis. Deregulation of post-translational modifications (PTMs) of proteins, especially phosphorylation, is present in many types of cancer. Therefore, the development of materials for the rapid sensing of low abundant phosphorylated peptides in biological samples can be of great therapeutic value. In this work, we have synthesised fluorescent molecularly imprinted polymers (fMIPs) for the detection of the phosphorylated tyrosine epitope of ZAP70, a cancer biomarker. The polymers were grafted as nanometer-thin shells from functionalised submicron-sized silica particles using a reversible addition-fragmentation chain-transfer (RAFT) polymerisation. Employing the combination of fluorescent urea and intrinsically cationic bis-imidazolium receptor cross-linkers, we have developed fluorescent sensory particles, showing an imprinting factor (IF) of 5.0. The imprinted polymer can successfully distinguish between phosphorylated and non-phosphorylated tripeptides, reaching lower micromolar sensitivity in organic solvents and specifically capture unprotected peptide complements in a neutral buffer. Additionally, we have shown the importance of assessing the influence of counterions present in the MIP system on the imprinting process and final material performance. The potential drawbacks of using epitopes with protective groups, which can co-imprint with targeted functionality, are also discussed.
KW - Functional monomers
KW - Molecularly imprinted polymers
KW - Phosphorylated peptides
KW - Fluorescence
KW - Core-shell particles
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588089
DO - https://doi.org/10.1039/d3tb01474f
SN - 2050-750X
SP - 1
EP - 10
PB - Royal Society of Chemistry
CY - Cambridge
AN - OPUS4-58808
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kleinbub, Sherin
A1 - Braymer, Joseph J
A1 - Pfeiffer, Friedhelm
A1 - Dyall-Smith, Mike
A1 - Spirgath, Kristin
A1 - Alfaro-Espinoza, Gabriela
A1 - Koerdt, Andrea
T1 - From Genes to Black Rust: Genomic insights into corrosive methanogens
N2 - Within the past ten years, genetic evidence has been increasing for the direct role that microbes play in microbiologically influenced corrosion (MIC), also known as biocorrosion or biodeterioration. One prominent example is the correlation between the corrosion of metal and the presence of genes encoding an extracellular [NiFe]-hydrogenase (MIC hydrogenase) in the methanogenic archaeon, Methanococcus maripaludis. In this study, DNA sequencing and bioinformatic analysis were used to classify the MIC hydrogenase as belonging to a core set of genes, the MIC core, found so far in Methanococci and Methanobacteria classes of methanogens. Genetic evidence is provided for the mobilization of the MIC core via multiple mechanisms, including a horizontal gene transfer event from Methanobacteria to Methanococci and a newly described MIC-transposon. A detailed comparison of M. maripaludis genomes further pointed to the relevance that cell wall modifications involving N-glycosylation of S-layer proteins and the MIC hydrogenase likely play in methanogen-induced MIC (Mi-MIC). Microscopic analysis of corrosive methanogens encoding the MIC core indicated that Methanobacterium-affiliated strain IM1 can form extensive biofilms on the surface of corrosion products whereas individual cells of M. maripaludis Mic1c10 were only found localized to crevices in the corrosion layer. An updated model of Mi-MIC involving two modes of action is presented, which predicts that the propensity of cells to adhere to iron surfaces directly influences the rate of corrosion due to the localization of the MIC hydrogenase at the metal-microbe interface.
KW - Biocorrosion
KW - Hydrogenases
KW - Metalloprotein
KW - Microbes
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649425
DO - https://doi.org/10.1093/femsmc/xtaf018
SN - 2633-6685
VL - 6
SP - 1
EP - 19
PB - Oxford University Press (OUP)
AN - OPUS4-64942
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Klinge, A
A1 - Mönig, J
A1 - Ziegert, C
A1 - Richter, Matthias
A1 - Kalbe, Ute
A1 - Horn, Wolfgang
A1 - Röhlen, U
A1 - Rauscher, S
A1 - Roswag-Klinge, E
T1 - upMIN 100 – upcycling of mineral construction and demolition waste to substitute natural aggregates in earthen building materials
N2 - The construction sector is one of the most resource-intensive sectors in Germany and is responsible for 40 % of CO2 emissions. Around 517 million tons of mineral raw materials are required annually for the construction of buildings in Germany. At the same time, mineral construction waste was the largest material flow at 229.3 million tons (2020). The rates of construction and demolition waste (CDW) recycling have increased since 2000, especially for mineral waste. Nevertheless, the majority of recycled aggregates are used in technically largely unregulated applications (e.g. road construction). This downcycling leads to a loss of valuable resources for technically and economically valuable applications. The upMIN 100 research project is investigating the question of whether and to what extent recycled CDW is suitable as an additive an binder in earthen building materials. The focus is placed on grain sizes of < 2 mm, which are currently predominantly landfilled, as there are at present no regulations for their use in building products. The soil matrix of earthen building materials however, naturally contains of different grain sizes, whith < 2mm – 0,063 for aggregates and < 0.063 mm as a binder. Therefore, the focused grain sizes (sand, clay and silt) could have a high usage potential. In order to enable the use of CDW, the technical feasibility must be ensured, quality requirements for source materials (e.g. threshold values for pollutants in terms of health and environmental compatibility and hazardous substances) and permissible proportions of recycled aggregates must be defined. Two different building material developments (earth blocks and -plaster)were used to assess both, the technical feasibility as well the pollutant content of the recycled aggregate and its final emissions into the indoor air. For both materials two mixtures could be established, that also meet the mechanical specifications according to the DIN standard, such as the compressive strength. A method was developed to design material mixtures with a high amount of CDW that comply with the defined limit values. The mixtures reached a recycling rate of 28 % with high mechanical properties and 70 % with minimum strength requirements.
KW - Mineral waste
KW - Upcycling
KW - Earthen building product
KW - Circular construction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652831
DO - https://doi.org/10.1088/1755-1315/1554/1/012084
SN - 1755-1307
VL - 1554
IS - 1
SP - 1
EP - 9
PB - IOP Publishing
AN - OPUS4-65283
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Knoche, Lisa
A1 - Lisec, Jan
A1 - Koch, Matthias
T1 - Analysis of electrochemical and liver microsomal transformation products of lasalocid by LC/HRMS
N2 - Rationale: Lasalocid (LAS), an ionophore, is used in cattle and poultry farming as feed additive for its antibiotic and growth-promoting properties. Literature on transformation products (TP) resulting from LAS degradation is limited. So far, only hydroxylation is found to occur as the metabolic reaction during the LAS degradation. To investigate potential TPs of LAS, we used electrochemistry (EC) and liver microsome (LM) assays to synthesize TPs, which were identified using liquid chromatography high-resolution mass spectrometry (LC/HRMS).
Methods: Electrochemically produced TPs were analyzed online by direct coupling of the electrochemical cell to the electrospray ionization (ESI) source of a Sciex Triple-TOF high resolution mass spectrometer. Then, EC-treated LAS solution was collected and analyzed offline using LC/HRMS to confirm stable TPs and improve their annotation with a chemical structure due to informative MS/MS spectra. In a complementary approach, TPs formed by rat and human microsomal incubation were investigated using LC/HRMS. The resulting data were used to investigate LAS modification reactions and elucidate the chemical structure of obtained TPs.
Results: The online measurements identified a broad variety of TPs, resulting from modification reactions like (de-)hydrogenation, hydration, methylation, oxidation as well as adduct formation with methanol. We consistently observed different ion complexations of LAS and LAS-TPs (Na+; 2Na+ K+; NaNH4 +; KNH4 +). Two stable methylated EC-TPs were found, structurally annotated, and assigned to a likely modification reaction. Using LM incubation, seven TPs were formed, mostly by oxidation/hydroxylation. After the identification of LM-TPs as Na+-complexes, we identified LM-TPs as K+-complexes.
Conclusion: We identified and characterized TPs of LAS using EC- and LM-based methods. Moreover, we found different ion complexes of LAS-based TPs. This knowledge, especially the different ion complexes, may help elucidate the metabolic and environmental degradation pathways of LAS.
KW - Mass Spectrometry
KW - Electrochemistry
KW - ECR
KW - Lasalocid
KW - Ionophore
KW - Transformation products
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553919
DO - https://doi.org/10.1002/rcm.9349
VL - 36
IS - 18
SP - 1
EP - 10
PB - Wiley online library
AN - OPUS4-55391
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Knoche, Lisa
A1 - Lisec, Jan
A1 - Schwerdtle, T.
A1 - Koch, Matthias
T1 - LC-HRMS-Based Identification of Transformation Products of the Drug Salinomycin Generated by Electrochemistry and Liver Microsome
N2 - The drug salinomycin (SAL) is a polyether antibiotic and used in veterinary Medicine as coccidiostat and growth promoter. Recently, SAL was suggested as a potential anticancer drug.
However, transformation products (TPs) resulting from metabolic and environmental degradation of SAL are incompletely known and structural information is missing. In this study, we therefore systematically investigated the formation and identification of SAL derived TPs using electrochemistry (EC) in an electrochemical reactor and rat and human liver microsome incubation (RLM and HLM) as TP generating methods. Liquid chromatography (LC) coupled to high-resolution mass spectrometry (HRMS) was applied to determine accurate masses in a suspected target analysis to identify TPs and to deduce occurring modification reactions of derived TPs. A total of 14 new, structurally different TPs were found (two EC-TPs, five RLM-TPs, and 11 HLM-TPs). The main modification reactions are decarbonylation for EC-TPs and oxidation (hydroxylation) for RLM/HLM-TPs. Of particular interest are potassium-based TPs identified after liver microsome incubation because these might have been overlooked or declared as oxidated sodium adducts in previous, non-HRMS-based studies due to the small mass difference between K and O + Na of 21 mDa. The MS fragmentation pattern of TPs was used to predict the position of identified modifications in the SAL molecule. The obtained knowledge regarding transformation reactions and novel TPs of SAL will contribute to elucidate SAL-metabolites with regards to structural prediction.
KW - Salinomycin
KW - Ionophore antibiotics
KW - Transformation product
KW - Electrochemistry
KW - Rat/human liver microsomes
KW - HRMS
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542543
DO - https://doi.org/10.3390/antibiotics11020155
SN - 2079-6382
VL - 11
IS - 2
SP - 155
PB - MDPI
CY - Basel
AN - OPUS4-54254
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Koch, Matthias
A1 - Mauch, Tatjana
A1 - Riedel, Juliane
T1 - Development of a Hydrazine-Based Solid-Phase Extraction and Clean-Up Method for Highly Selective Quantification of Zearalenone in Edible Vegetable Oils by HPLC-FLD
N2 - Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the Fusarium mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47–494 μg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part).
KW - Mycotoxin
KW - Food
KW - Reversible covalent hydrazine chemistry (RCHC)
KW - Quantitative determination
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554812
DO - https://doi.org/10.3390/toxins14080549
VL - 14
IS - 8
PB - MDPI
CY - Basel
AN - OPUS4-55481
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kornev, Roman
A1 - Gornushkin, Igor B.
A1 - Shabarova, Lubov
A1 - Kadomtseva, Alena
A1 - Mochalov, Georgy
A1 - Rekunov, Nikita
A1 - Romanov, Sergey
A1 - Medov, Vitaly
A1 - Belousova, Darya
A1 - Maleev, Nikita
T1 - Plasma-Chemical Disposal of Silicon and Germanium Tetrachlorides Waste by Hydrogen Reduction
N2 - The processes of hydrogen reduction of silicon and germanium chlorides under the conditions of high-frequency (40.68 MHz) counteracted arc discharge stabilized between two rod electrodes are investigated. The main gas-phase and solid products of plasma-chemical transformations are determined. Thermodynamic analysis of SiCl4 + H2 and GeCl4 + H2 systems for optimal process parameters was carried out. Using the example of hydrogen reduction of SiCl4 by the method of numerical modeling, gas-dynamic and thermal processes for this type of discharge are investigated. The impurity composition of gas-phase and solid reaction products is investigated. The possibility of single-stage production of high-purity Si and Ge mainly in the form of compact ingots, as well as high-purity chlorosilanes and trichlorogermane, is shown.
KW - High-frequency arc discharge
KW - Hydrogen reduction
KW - Silicon chlorides
KW - Germanium chlorides
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594454
DO - https://doi.org/10.3390/sci6010001
VL - 6
IS - 1
SP - 1
EP - 12
PB - MDPI AG
AN - OPUS4-59445
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kossatz, Philipp
A1 - Mezhov, Alexander
A1 - Andresen, Elina
A1 - Prinz, Carsten
A1 - Schmidt, Wolfram
A1 - Resch-Genger, Ute
T1 - Assessing the Applicability of Lanthanide-Based Upconverting Nanoparticles for Optically Monitoring Cement Hydration and Tagging Building Materials
N2 - Chemically stable, lanthanide-based photon upconversion micro- and nanoparticles (UCNPs) with their characteristic multicolor emission bands in the ultraviolet (UV), visible (vis), near-infrared (NIR), and short-wave infrared (SWIR) arepromising optical reporters and barcoding tags. To assess the applicability of UCNPs for the monitoring of early stage cement hydration processes and as authentication tags for cementitious materials, we screened the evolution of the luminescence of Selfmade core-only NaYF4:Yb,Er UCNPs and commercial μm-sized Y2O2S:Yb,Er particles during the first stages of cement hydration, which largely determines the future properties of the hardened material. Parameters explored from the UCNP side included particle size, morphology, surface chemistry or coating, luminescence properties, and concentration in different cement mixtures. From the cement side, the influence of the mineral composition of the cement matrix was representatively examined for ordinary Portland cement (OPC) and its constituents tricalcium aluminate (C3A), tricalcium silicate (C3S), and gypsum at different water to cement ratios. Based on reflection and luminescence measurements, enabling online monitoring, which were complemented by XRD and isothermal heat-flow calorimetric measurements to determine whether the incorporation of these particles could impair cement hydration processes, well suited lanthanide particle reporters could be identified as well as application conditions. In addition, thereby the reporter influence on cement hydration kinetics could be minimized while still preserving a high level of information content. The best performance for the luminescence probing of changes during early stage cement hydration processes was observed for 25 nm-sized oleate (OA)-coated UCNPs added in a concentration of 0.1 wt %. Higher UCNP amounts of 1.0 wt % delayed cement hydration processes size- and surface coatingspecifically in the first 24 h. Subsequent luminescence stability screening studies performed over a period of about one year support the applicability of UCNPs as optical authentication tags for construction materials.
KW - Quality assurance
KW - Fluorescence
KW - Nano
KW - Particle
KW - Synthesis
KW - Quantum yield
KW - NIR
KW - Mechanism
KW - Characterization
KW - XRD
KW - Calorimetry
KW - Advanced material
KW - Cement
KW - Monitoring
KW - Surface
KW - Size
KW - Lifetime
KW - Barcode
KW - Lanthanide
KW - Upconversion
KW - Encoding
KW - Method
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638318
DO - https://doi.org/10.1021/acsomega.5c02236
SN - 2470-1343
VL - 10
IS - 29
SP - 31587
EP - 31599
PB - ACS Publications
CY - Washington, DC
AN - OPUS4-63831
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kowalewska, Z.
A1 - Abad Andrade, Carlos Enrique
A1 - Okruss, M.
A1 - Recknagel, Sebastian
T1 - Feasibility of high-resolution continuum source molecular absorption spectrometry for vanadium determination
N2 - This work aimed to evaluate high-resolution continuum source molecular absorption spectrometry (HR-CS MAS), traditionally used to determine non-metals, for the determination of a new element, metal, vanadium. VO was selected as a target molecule because it is relatively stable and was expected to be spontaneously generated in a flame or a graphite furnace (GF). The high-resolution overview spectra of the molecule were obtained in a wide range of 480–630 nm, and absorption due to the X4Σ−–C4Σ− electronic transition was registered. A unique instrumental setup, comprising a prototype Modular Simultaneous Echelle Spectrograph (MOSES) and a commercial HR-CS MAS apparatus, was applied in the research. Finally, the spectral area centered at 550.6230 nm was selected for analysis. A method was developed to determine V in solutions of catalysts of heavy petroleum oil hydroprocessing using a commercial HR-CS spectrometer in a flame version. Although sensitivity was relatively poor (characteristic concentration 380 mg L−1), an extremely low noise enabled reaching a satisfactory detection limit (20 mg L−1 in solution, i.e. 0.1% m:m in the catalyst). For the first time vanadium was determined using ordinary air-acetylene flame. The obtained results were consistent with the results of atomic absorption spectrometry with N2O-C2H2 flame. Unfortunately, only a small population of VO molecules could have been generated in GF measurements. Furthermore, the observed VO molecules appeared only at unfavorably high temperatures. The work shows the potential of HR-CS MAS as a scientific tool for investigating the mechanism of processes occurring in the GF. This work can inspire other research of new analytes for HR-CS MAS.
KW - Vanadium
KW - HR-CS-MAS
KW - VO
KW - High-resolution continuum source molecular absorption spectrometry
KW - AAS
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569899
DO - https://doi.org/10.1039/D2JA00281G
SN - 0267-9477
VL - 38
IS - 2
SP - 472
EP - 483
PB - Royal Society of Chemistry
AN - OPUS4-56989
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Krahl, T.
A1 - Beer, F.
A1 - Relling, A.
A1 - Gawlitza, Kornelia
A1 - Rurack, Knut
A1 - Kemnitz, E.
T1 - Toward Luminescent Composites by Phase Transfer of SrF2 :Eu3+ Nanoparticles Capped with Hydrophobic Antenna Ligands
N2 - Transparent dispersions of hydrophobic SrF2 :Eu3+ nanoparticles in cyclohexane with up to 20% europium were obtained by fluorolytic sol-gel synthesis followed by Phase transfer into cyclohexane through capping with sodium dodecylbenzenesulfonate (SDBS). The particles were characterized by TEM, XRD and DLS as spherical objects with a diameter between 6 and 11 nm in dry state. 1H-13CP MAS NMR experiments revealed the binding of the anionic sulfonate head group to the particle surface. The particles show bright red luminescence upon excitation of the aromatic capping agents, acting as antennas for an Energy transfer from the benzenesulfonate unit to the Eu3+ centers in the particles. This synthesis method overcomes the current obstacle of the fluorolytic sol-gel synthesis that transparent dispersions can be obtained directly only in hydrophilic solvents. To demonstrate the potential of such hydrophobized alkaline-earth fluoride particles, transparent luminescent organic-inorganic composites with 10% SrF2 :Eu3+ embedded into polyTEGDMA, polyBMA, poly-BDDMA and polyD3MA, respectively, were prepared, endowing the polymers with the luminescence features of the nanoparticles.
KW - Nanoparticles
KW - Fluorides
KW - Sol-gel process
KW - Organic-inorganic hybrid composites
PY - 2020
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508668
DO - https://doi.org/10.1002/cnma.202000058
SP - 1
EP - 11
PB - Wiley
AN - OPUS4-50866
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Krappe, Alexander R.
A1 - Mayer, Jacob C.
A1 - Zhang, Wuai
A1 - Filla, Lina M.
A1 - Ligorio, Giovanni
A1 - Hermerschmidt, Felix
A1 - Eitelhuber, Larissa S.
A1 - Güttler, Arne
A1 - Weber, Manuela
A1 - Paulus, Beate
A1 - Resch-Genger, Ute
A1 - List-Kratochvil, Emil J.W.
A1 - Eigler, Siegfried
T1 - Highly Emissive Hexa-peri-benzocoronene-fluoranthene Hybrid as Easily Processable and Stable OLED Material
N2 - We report the synthesis of a fluorescent polycyclic aromatic hydrocarbon dye with a “symmetry-broken” core, derived from the related hexa-peri-benzocoronene (HBC) core with fluoranthene subunit. The fluorophore is composed of a pure Carbon skeleton without heteroatoms and exhibits remarkable photo luminescence properties with a photoluminescence Quantum yield (PLQY) of up to 67% in toluene, exceeding that of theparent HBC by a factor of 30. The single crystal X-ray structure reveals the distorted polycyclic aromatic hydrocarbon structure, which is responsible for the optoelectronic properties, as supported by density functional theory calculations. We show that the new fluorescent dye can be readily used for the fabrication of organic light-emitting diodes (OLED) without extensive optimization, whereby solubility in a variety of solvents and successful film formation are decisive.
KW - Quantum Yield
KW - OLED
KW - Fluorescence
KW - Synthesis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631298
DO - https://doi.org/10.1002/chem.202500742
SN - 1521-3765
SP - 1
EP - 7
PB - John Wiley & Sons, Inc
AN - OPUS4-63129
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -