TY - JOUR A1 - Kittler, Katrin A1 - Hoffmann, Holger A1 - Lindemann, Franziska A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, Ronald T1 - Biosynthesis of 15N-labeled cylindrospermopsin and its application as internal standard in stable isotope dilution analysis N2 - Cylindrospermopsin (CYN) is a cyanobacterial toxin associated with human and animal poisonings. Due to its toxicity in combination with its widespread occurrence, the development of reliable methods for selective, sensitive detection and accurate quantification is mandatory. Liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis using stable isotope dilution analysis (SIDA) represents an ideal tool for this purpose. U-[15N5]-CYN was synthesized by culturing Aphanizomenon flos-aquae in Na15NO3-containing cyanobacteria growth medium followed by a cleanup using graphitized carbon black columns and mass spectrometric characterization. Subsequently, a SIDA-LC-MS/MS method for the quantification of CYN in freshwater and Brassica matrices was developed showing satisfactory performance data. The recovery ranged between 98 and 103 %; the limit of quantification was 15 ng/L in freshwater and 50 µg/kg dry weight in Brassica samples. The novel SIDA was applied for CYN determination in real freshwater samples as well as in kale and in vegetable mustard exposed to toxin-containing irrigation water. Two of the freshwater samples taken from German lakes were found to be CYN-contaminated above limit of quantification (17.9 and 60.8 ng/L). CYN is systemically available to the examined vegetable species after exposure of the rootstock leading to CYN mass fractions in kale and vegetable mustard leaves of 15.0 µg/kg fresh weight and 23.9 µg/kg fresh weight, respectively. CYN measurements in both matrices are exemplary for the versatile applicability of the developed method in environmental analysis. KW - Cyanotoxin KW - Quantification KW - Surface water KW - Vegetable plants KW - SIDA KW - HPLC-MS/MS PY - 2014 DO - https://doi.org/10.1007/s00216-014-8026-y SN - 1618-2642 SN - 1618-2650 VL - 406 IS - 24 SP - 5765 EP - 5774 PB - Springer CY - Berlin AN - OPUS4-31566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Mineralölkohlenwasserstoffen mittels GC-FID in verschiedenen Matrices T2 - Analytikertreffen 2000 der DGMK CY - Hamburg, Germany DA - 2000-11-13 PY - 2000 AN - OPUS4-5754 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Wachholz, Sigrid A1 - Win, Tin A1 - Nehls, Irene T1 - Analytik von Mineralölkohlenwasserstoffen: Die Problematik der Probenaufbereitung KW - Adsorbentien KW - Aromatische Verbindungen KW - Wiederfindung KW - Extraktionsmittel KW - Böden KW - MKW-Bestimmung KW - Mineralölkohlenwasserstoffe (MKW) KW - Mineralölkohlenwasserstoffe KW - Analytik KW - n-Alkane KW - Wiederfindung KW - Polare Verbindungen PY - 1998 SN - 0934-3504 SN - 1865-5084 VL - 10 IS - 5 SP - 265 EP - 270 PB - Springer CY - Heidelberg AN - OPUS4-7040 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Die Bestimmung von Phomopsin A in Leguminosen mittels Stabilisotopenverdünnungsanalyse T2 - 44. Deutscher Lebensmittelchemikertag CY - Karlsruhe DA - 2015-09-14 PY - 2015 AN - OPUS4-34673 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Buge, Hans-Gerhard A1 - Becker, Roland A1 - Nehls, Irene T1 - Kalibrierstandard für die Mineralöl (MKW)-analytik mittels GC-FID KW - Kalibrierstand KW - Referenzmaterial KW - MKW KW - GC PY - 2005 SN - 0016-3538 VL - 49 IS - 11 SP - 207 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-11601 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Development of certified reference material and analytical method for zearalenone in edible oil N2 - Quality and safety of food products require their reliable analysis. Contaminants, in particular mycotoxins, are key-components for food safety. About 25 % of the world's food crops are contaminated with mycotoxins posing a severe health risk to humans. In order to strengthen food safety and consumer protection the European Commission (EC) set maximum levels for priority mycotoxins in certain foods for human consumption. In 2013, the EC and CEN (European Committee for Standardization) started an initiative to standardize analytical methods for mycotoxins in food which gained increasing relevance, e.g. zearalenone (ZEN). ZEN, an estrogenic mycotoxin produced by several Fusarium species, contaminates cereal crops worldwide. Due to its lipophilic nature ZEN is often found in edible oils (particularly in maize germ oils) derived from contaminated plants. Therefore, an European maximum level of 400 µg/kg is currently in force. To perform reliable food analysis a sustainable metrological infrastructure is of major importance enabling the quantification of priority mycotoxins (here: ZEN). To achieve this goal, an integrated approach is needed targeted at the development of validated analytical methods and certified reference materials (CRM). A highly selective method for ZEN in edible oils will be presented, based on solid phase extraction (SPE) using hydrazine-functionalized particles. This method was developed for manual application using commercial SPE cartridges as well as for automated SPE-HPLC online coupling. While ZEN is covalently coupled to the solid phase by means of a hydrazone bond, undesired matrix components can be removed very efficiently. Finally, ZEN is decoupled from the solid phase, leading to highly purified extracts which are measured by HPLC-FLD. The development of the first European Reference Material (ERM®) for ZEN in maize germ oil (ERM®-BC715) will be presented and discussed. This ERM®-project underpins the urgent need for mycotoxin-CRMs to support food safety and public health. T2 - 40. Generalversammlung ISO/REMCO CY - Berlin, Germany DA - 27.06.2017 KW - Certified reference materials KW - Mycotoxin KW - Food PY - 2017 AN - OPUS4-40902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Rasenko, Tatjana A1 - Merkel, Stefan A1 - Mönch, Bettina A1 - Koch, Matthias T1 - Novel solid-phase extraction for epimer-specific quantification of ergot alkaloids in rye flour and wheat germ oil N2 - Ergot alkaloids and their epimer-specific determination have gained increasing importance for food safety. A solid-phase extraction and cleanup method based on sodium-neutralized strong cation exchange (Na+-SCX) was developed to quantitate 12 priority ergot alkaloids in rye flour and wheat germ oil by HPLC fluorescence analysis. Sample preparation is achieved by omitting acidic and alkaline conditions enabling minimized epimerization, which is necessary to determine ergot alkaloids according to their natural distribution in foods. Ergot alkaloids are eluted from SCX-column by forming ion pairs using a sodium hexanesulfonate containing solution which prevents epimerization for at least 96 h. Method validation yielded recoveries of 80–120% (rye flour) and 71–96% (wheat germ oil) with a maximum limit of quantitation (LOQ) of 2.0 µg kg–1 per ergot alkaloid for both matrices. The applicability of the developed method was demonstrated by analyzing 16 samples from German retail markets: 9 rye flours (max 178 ± 5 µg kg–1) and, reported for the first time, 7 wheat germ oils (max 56.8 ± 2.7 µg kg–1) expressed as the sum of 12 ergot alkaloids. KW - Sample preparation KW - SCX-resin KW - Isomerization KW - Vegetable oil KW - Rye flour KW - HPLC PY - 2013 DO - https://doi.org/10.1021/jf403628q SN - 0021-8561 SN - 1520-5118 VL - 61 IS - 45 SP - 10699 EP - 10707 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-29592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Köppen, Robert A1 - Nehls, Irene T1 - Neue Mykotoxin-Referenzmaterialien - Qualitätssicherung in der Lebensmittelanalytik N2 - Die zuverlässige Überwachung geltender Mykotoxin-Grenzwerte ist elementarer Bestandteil von Lebensmittelsicherheit und Verbraucherschutz. Durch die zunehmende Bedeutung der Qualitätssicherung ist auch die Nachfrage an zertifizierten Referenzmaterialien (ZRM) in den letzten Jahren deutlich gestiegen. Dem steht derzeit jedoch nur eine sehr begrenzte Auswahl geeigneter ZRM gegenüber. KW - Zertifiziertes Referenzmaterial KW - ERM KW - Ochratoxin A KW - Deoxynivalenol KW - Nivalenol KW - Zearalenon KW - Kaffee KW - Wein KW - Weizen PY - 2011 SN - 0012-0413 SN - 1869-2214 IS - September SP - 434 EP - 448 PB - Wiss. Verl.-Ges. CY - Stuttgart AN - OPUS4-24616 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Riedel, Juliane A1 - Emmerling, Franziska A1 - Koch, Matthias T1 - (3S,11Z)-14,16-dihydroxy-3-methyl-3,4,5,6,9,10-hexahydro-1H-2-benz-oxacyclotetradecine-1,7(8H)-dione (cis-zearalenone): a redetermination N2 - The title compound, also known as cis-zearalenone (cis-ZEN), C18H22O5, has already been reported elsewhere [Griffin et al. (1981). ACA Ser. 29, 35], but no atomic coordinates are publicly available. The molecule is of interest with respect to its toxicity. In the crystal, intramolecular O—H···O hydrogen bonds stabilize the molecular conformation, while intermolecular O—H···O hydrogen bonds link the molecules to form infinite chains along the [110] and [1¯10] directions. The absolute configuration has been assigned by reference to an unchanging chiral centre in the synthetic procedure. PY - 2012 DO - https://doi.org/10.1107/S1600536812002735 SN - 1600-5368 VL - 68 IS - 3 SP - o832, sup1 EP - sup8 PB - Munksgaard CY - Copenhagen AN - OPUS4-25546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Zearalenone in edible oil - a method comparison study T2 - 33. Mykotoxin-Workshop der Gesellschaft für Mykotoxinforschung e. V. CY - Freising, Germany DA - 2011-05-30 PY - 2011 N1 - Geburtsname von Sauer, Andreas: Buchholz, A. - Birth name of Sauer, Andreas: Buchholz, A. AN - OPUS4-23506 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Bremser, Wolfram A1 - Rasenko, Tatjana A1 - Koch, Matthias T1 - Development and certification of a reference material for Fusarium mycotoxins in wheat flour N2 - Deoxynivalenol (DON), nivalenol (NIV) and zearalenone (ZEN) are toxic secondary metabolites produced by several species of Fusarium fungi. These mycotoxins are often found together in a large variety of cereal-based foods, which are regulated by maximum content levels of DON and ZEN. To date, suitable certified reference materials (CRM) intended for quality control purposes are lacking for these Fusarium mycotoxins. In order to overcome this lack, the first CRM for the determination of DON, NIV and ZEN in naturally contaminated wheat flour (ERM®-BC600) was developed in the framework of a European Reference Materials (ERM®) project. This article describes and discusses the whole process of ERM®-BC600 development, including material preparation, homogeneity and stability studies, and an interlaboratory comparison study for certification. A total of 21 selected expert laboratories from different European countries with documented expertise in the field of mycotoxin analysis took part in the certification study using various gas and liquid chromatographic methods. The certified values and their corresponding expanded uncertainties (k=2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows: 102±11 µgkg-1 for DON, 1000±130 µgkg-1 for NIV and 90±8 µgkg-1 for ZEN. KW - Deoxynivalenol KW - Nivalenol KW - Zearalenone KW - Food KW - ERM KW - Quality assurance PY - 2013 DO - https://doi.org/10.1007/s00216-013-6857-6 SN - 1618-2642 SN - 1618-2650 VL - 405 IS - 14 SP - 4755 EP - 4763 PB - Springer CY - Berlin AN - OPUS4-28303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Lisec, Jan A1 - Sommerfeld, Thomas A1 - Riedel, Juliane A1 - Mauch, Tatjana A1 - Koch, Matthias T1 - CRM BAM-B003 eCerto data file N2 - Data file (RData) containing measurement data recorded during the production process of the Certified Reference Material BAM-B003 containing per- and polyfluoroalkyl substances (PFAS) in textiles. The data can be most conveniently openend using the Shiny-App eCerto which is accessible at https://www.bam.de/eCerto. KW - Certified reference material KW - Mass spectrometry KW - PFAS PY - 2025 DO - https://doi.org/10.5281/zenodo.15907581 PB - Zenodo CY - Geneva AN - OPUS4-64544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Entwicklung von Analysenverfahren, Standards und Referenzmaterialien für die Lebensmittelanalytik N2 - Mykotoxine gehören weltweit zu den am meisten untersuchten Kontaminanten in Lebensmitteln. Ihre zuverlässige Bestimmung ist zur Kontrolle geltender Grenzwerte notwendig und erfordert die Verfügbarkeit reiner Kalibrierstandards, valider Analysenverfahren sowie (zertifizierter) Referenzmaterialien. Im Vortrag werden die aktuellen Aktivitäten der BAM hinsichtlich der Entwicklung von Standards, Analysenverfahren und Referenzmaterialien für die Mykotoxin-Analytik vorgestellt. T2 - Netzwerk Diagnostik Berlin-Brandenburg e.V. CY - Berlin, Germany DA - 29.06.2016 KW - Mykotoxine KW - Lebensmittel KW - Qualitätssicherung PY - 2016 AN - OPUS4-38862 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maul, Ronald A1 - Dahmen-Levison, U. A1 - Koch, Matthias T1 - Mykotoxin-Cleanup mit Spin-Säulen - Evaluierung der Leistungsfähigkeit neuer Zentrifugationssäulen für die Analyse der Trichothecen-Mykotoxine DON, D3G, T2- und HT2-Toxin N2 - Mykotoxine sind toxische, von Schimmelpilzen gebildete Sekundärstoffe und gehören zu den am weitesten verbreiteten Lebensmittelkontaminanten. Trichtothecen-Mykotoxine, produziert von verschiedenen Fusarien-Spezies, sind dabei aufgrund ihrer hohen akuten Toxizität teils im Lebensmittel mit Grenzwerten geregelt oder befinden sich aktuell in einer entsprechenden Diskussion. PY - 2013 SN - 0012-0413 SN - 1869-2214 VL - 109 IS - März SP - 131 EP - 138 PB - Wiss. Verl.-Ges. CY - Stuttgart AN - OPUS4-28697 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weiz, S. A1 - Marten, S. A1 - Heinze, J. A1 - Drzymala, Sarah A1 - Koch, Matthias T1 - Zearalenon auf der Spur - Hochselektive Mykotoxin-Bestimmung in Speiseöl N2 - Das neue Verfahren ermöglicht die direkte Analyse des Mykotoxins Zearalenon aus Speiseölen in Kombination mit einer hochselektiven Probenvorbereitung. Dies wird in einem automatisierten Online-SPE-HPLC-Prozess abgebildet, sodass ene routinemäßige Kontrolle des EU-Grenzwertes möglich ist. KW - Mykotoxine KW - HPLC KW - Online-SPE KW - Hydrazine PY - 2014 SN - 0012-0413 SN - 1869-2214 IS - Januar SP - 24 EP - 27 PB - Wiss. Verl.-Ges. CY - Stuttgart AN - OPUS4-30080 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Development of Certified Reference Materials for the determination of mineral oil hydrocarbons in water, soil and waste T2 - BERM 9 - 9th International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 2003-06-15 PY - 2003 AN - OPUS4-4788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - New reference materials for mycotoxins and acrylamide - perfect tools for reliable food analysis T2 - Tag der Chemie, FU Berlin CY - Berlin, Germany DA - 2010-06-16 PY - 2010 AN - OPUS4-21307 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Rita A1 - Koch, Matthias A1 - Nehls, Irene T1 - Ringversuch für Acrylamid, Theobromin und Coffein in Kakao KW - Ringversuch KW - Acrylamid KW - Theobromin KW - Coffein KW - Kakao PY - 2008 SN - 0937-1478 SN - 1521-3811 VL - 62 IS - 4 SP - 110 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-17848 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Traub, Heike A1 - Koch, Matthias A1 - Lück, Detlef A1 - Win, Tin A1 - Lehnik-Habrink, Petra A1 - Schultze, Karin A1 - Saring, U. A1 - Plagemann, R. T1 - Evaluierung von Verfahren für die Untersuchung von Böden nach § 8 Bundes-Bodenschutzgesetz (BBodSchG) (Forschungsbericht 299 71 224 / UBA-FB 000303) N2 - Evaluation of methods for the analysis of soils according to § 8 of the German Federal Soil Protection Act (BBodSchG) The German Federal Soil Protection Act establishes the conditions for effective soil protection and remediation of contaminated sites. In the German Federal Soil Protection and Contaminated Sites Ordinance (BBodSchV) limiting values and methods for the determination of environmentally harmful substances in soils are fixed. The aim of this project was to evaluate selected methods by comparative investigations and proficiency testing schemes. New methods for the determination of inorganic and organic pollutants should be developed and compared with the existing standard methods. Despite the widespread use of ICP-OES up to now no national or international standard is available for the determination of heavy metals in soil extracts with this analytical method. The influence of spectral and non spectral interferences on the accuracy of the results was systematically investigated, especially based on aqua regia soil extracts. Analyte concentration equivalents were determined, too. Based on these results a proposal for a standard was submitted to the corresponding working group of ISO TC 190.[...] KW - Evaluierung von Analyseverfahren KW - ICP-OES KW - Chrom(VI) KW - Cyanide KW - Säulenelution KW - Bodenluft KW - Vor-Ort-Analytik KW - PAK KW - OCP KW - PCB KW - PCP KW - Referenzmaterialien KW - Messunsicherheit PY - 2002 UR - http://www.umweltbundesamt.de/publikationen/evaluierung-von-verfahren-fuer-untersuchung-von SN - 1862-4804 SN - 0722-186X IS - 32 SP - 1 EP - 339 PB - Umweltbundesamt CY - Dessau-Roßlau AN - OPUS4-1760 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sebald, M. A1 - Gebauer, J. A1 - Koch, Matthias T1 - Diastereoselective synthesis of (±)-trichodiene and (±)-trichodiene-D3 as analytical standards for the on-site quantification of trichothecenes N2 - The ubiquitous Fusarium genus is responsible for the spoilage of vast amounts of cereals and fruits. Besides the economic damage, the danger to human and animal health by the concomitant exposure to mycotoxins represents a serious problem. A large number of Fusarium species produce a variety of different mycotoxins of which the class of trichothecenes are of particular importance due to their toxicity. Being identified as the common volatile precursor during the biosynthesis of trichothecenes, (−)-trichodiene (TD) is considered to be a biomarker for the respective mycotoxin content in food samples. We postulated that the development of a non-invasive, on-site GC-IMS method for the quantification of (−)-trichodiene supplemented with a stationary SIDA headspace GC-MS reference method would allow circumventing the laborious and expensive analyses of individual trichothecenes in large cereal samples. In this work we present the syntheses of the required native calibration standard and an isotope labeled (TD-D3) internal standard. KW - Mycotoxins KW - Volatile marker KW - Food analysis KW - Screening method KW - Mobile analysis PY - 2021 DO - https://doi.org/10.1039/d1ob01778k VL - 19 IS - 45 SP - 9872 EP - 9879 PB - RSC AN - OPUS4-53993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Koch, Matthias A1 - Nehls, Irene T1 - Überwachung pflanzlicher Rohstoffe - Trichothecen-Analytik in Getreide und Getreideerzeugnissen PY - 2010 SN - 0012-0413 SN - 1869-2214 VL - 106 IS - DLR Spezial 2 SP - 66 EP - 72A PB - Wiss. Verl.-Ges. CY - Stuttgart AN - OPUS4-22206 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sommerfeld, Thomas A1 - Koch, Matthias T1 - CRM candidate for PAH mass fractions in rubber toys N2 - Polycyclic aromatic hydrocarbons (PAH) can contaminate plastic and rubber parts of consumer products including toys. PAH are present as impurities in some of the raw materials used for production of such articles, particularly in extender oils and in carbon black. Because PAH have negative effects on health (e.g. carcinogenic), standard methods have been developed in several countries to control PAH in consumer/toy products, mainly based on gas-chromatography mass-spectrometry (GC-MS). To protect consumers from hazards of PAH, national regulations and maximum levels are already in force, for example in Germany. Recently, maximum levels for 8 PAH compounds (benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[j]fluoranthene, benzo[e]pyrene, benzo[a]pyrene and dibenz[a,h]anthracene) have been established by EC-regulation 1272/2013. This resulted in an urgent need for certified reference materials (CRM) to meet the requirements of the EC-regulation (1 mg/kg for each PAH compound in consumer products and 0.5 mg/kg in toys, respectively). In 2016 BAM started a project to certify the PAH mass fractions in a toy CRM to fill the current gap of available reference materials. Several different toys from retailers were screened to obtain a real-life material representing PAH mass fractions in the range of the EC-maximum level. The finally selected material (rubber balls for children) was prepared and characterized with respect to homogeneity and stability of 18 PAH. The extension to other health-relevant PAH compounds, e.g. indeno[1,2,3-cd]pyrene and benzo[ghi]perylene, will increase the applicability of the CRM for costumers, e.g. from industry, conformity assessment bodies and private testing laboratories. The poster will present the current status of the ongoing CRM project including preparation of the candidate material and results from homogeneity and stability studies. In addition, first results of a joint German-Chinese interlaboratory comparison study will be shown. T2 - BERM-15, International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 23.09.2018 KW - Reference material KW - Organic contaminants KW - Toys KW - REACH PY - 2018 AN - OPUS4-46114 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siegel, David A1 - Merkel, Stefan A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - 3-{1-[(2,4-Dinitrophenyl)hydrazino]ethylidene}-5-(1-methylpropyl)pyrrolidine-2,4-dione KW - Tenuazonic acid 2,4-dinitrophenylhydrazone KW - X-ray single crystal diffraction KW - Crystal structure PY - 2009 DO - https://doi.org/10.1107/S1600536809012458 SN - 1600-5368 VL - 65 IS - 5 SP - o988 EP - o989 PB - Munksgaard CY - Copenhagen AN - OPUS4-19736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klaus, Christian A1 - Soruco Aloisio, Ricardo A1 - Koch, Claudia A1 - Prellwitz, Matthias T1 - Towards Safety and Accuracy of Hydrogen Refuelling Stations through Digital Twins N2 - This paper presents digital quality infrastructure methods for hydrogen refueling stations using the Asset Administration Shell as a standardized digital twin. Implemented at BAM’s test platform, it integrates real-time sensor data, calibration certificates, and compliance documents to support traceable, interoperable asset management. In combination with AI and semantic tools, the system will enable predictive maintenance, remote audits, and improved safety. This approach reduces downtime, enhances transparency, and offers a scalable model demonstrating the potential of digital twins in advancing metrological traceability and operational efficiency in hydrogen technologies. T2 - IMEKO TC-6 International Conference on Metrology and Digital Transformation - M4DConf 2025 CY - Benevento, Italy DA - 03.09.2025 KW - Datenintregration KW - IT KW - Verwaltungsschale KW - Infrastruktur KW - OT KW - Open Source KW - Software PY - 2025 UR - https://www.m4dconf.org/ UR - https://www.sciencedirect.com/journal/measurement-digitalization SP - 1 EP - 6 AN - OPUS4-64951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schloß, S. A1 - Hackl, T. A1 - Herz, C. A1 - Lamy, E. A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, R. T1 - Detection of a Toxic Methylated Derivative of Phomopsin A Produced by the Legume-Infesting Fungus Dioporthe toxica N2 - Phomopsin A (PHO-A), produced by the fungus Diaporthe toxica, is a mycotoxin known to be responsible for fatal liver disease of lupin-fed sheep. The füll spectrum of the toxic secondary metabolites produced by D. toxica is still unknown. PHO-A and the naturally occurring derivatives B—E have been subject to several studies to reveal their structures as well as chemical and toxicological properties. In this work, a methylated derivative of PHO-Aisolated firom lupin seeds inoculated %vith D. toxica is described. It was characterized by high-resolution mass and NMR data and shown to be the N-methylated derivative of PHO-A 1 is cytotoxic againstHepG2 cells. KW - Mycotoxins KW - Identification KW - Food PY - 2017 DO - https://doi.org/10.1021/acs.jnatprod.6b00662 VL - 80 IS - 6 SP - 1930 EP - 1934 PB - ACS Publications AN - OPUS4-41116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Temgoua, Ranil C.T. A1 - Lisec, Jan A1 - Koch, Matthias T1 - Recent Advances in Electrochemical Analysis of Phenylurea Herbicides N2 - Phenylurea herbicides (PUHs) are extensively used in modern agriculture due to their high efficiency in weed control; however, their widespread application has led to persistent environmental contamination and growing public health concerns. Reliable, sensitive, and selective analytical methods are therefore essential for monitoring these compounds in environmental and food matrices. Although several recent reviews have addressed electrochemical sensors and biosensors for a broad range of pollutants, there is currently no dedicated review focusing exclusively on PUHs while integrating electrochemical sensors, biosensors, molecularly imprinted polymers (MIPs), and electrochemical detection coupled with liquid chromatography (LC). This review provides a comprehensive and critical overview of electrochemical strategies developed for the analysis of PUHs. Core electroanalytical techniques, including cyclic voltammetry (CV), differential pulse voltammetry (DPV), square wave voltammetry (SWV), and chronoamperometry (CA), are discussed in terms of their fundamental principles, analytical roles, and suitability for mechanistic investigation, quantitative determination, and rapid screening. Electrochemical impedance spectroscopy (EIS) is also examined, particularly for its application in the characterization of electrode interfaces and in electrochemical biosensor development. Furthermore, the integration of electrochemical methods with mass spectrometry is highlighted as a powerful approach for elucidating redox mechanisms and identifying electrochemical transformation products. More than one hundred electrochemical sensors and biosensors reported between 1993 and 2025 are critically evaluated, with emphasis on electrode materials, surface modification strategies, detection mechanisms, analytical performance, and applicability to real samples. The advantages and limitations of electrochemical sensors, biosensors, and MIP-based platforms are systematically discussed in the context of sensitivity, selectivity, response time, and matrix effects. By synthesizing current advances and identifying remaining challenges, this review aims to provide clear guidance for future research and to support the development of robust, efficient, and application-oriented electrochemical methods for PUHs analysis. KW - Mass Spectrometry KW - Phenylurea herbicides KW - Electrochemistry PY - 2025 DO - https://doi.org/10.1016/j.snr.2025.100431 SN - 2666-0539 VL - 11 SP - 1 EP - 67 PB - Elsevier B.V. AN - OPUS4-65286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drzymala, Sarah A1 - Weiz, S. A1 - Heinze, J. A1 - Marten, S. A1 - Prinz, Carsten A1 - Zimathies, Annett A1 - Garbe, L.-A. A1 - Koch, Matthias T1 - Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil N2 - Established maximum levels for the mycotoxin zearalenone (ZEN) in edible oil require monitoring by reliable analytical methods. Therefore, an automated SPE-HPLC online system based on dynamic covalent hydrazine chemistry has been developed. The SPE step comprises a reversible hydrazone formation by ZEN and a hydrazine moiety covalently attached to a solid phase. Seven hydrazine materials with different properties regarding the resin backbone, pore size, particle size, specific surface area, and loading have been evaluated. As a result, a hydrazine-functionalized silica gel was chosen. The final automated online method was validated and applied to the analysis of three maize germ oil samples including a provisionally certified reference material. Important performance criteria for the recovery (70–120 %) and precision (RSDr <25 %) as set by the Commission Regulation EC 401/2006 were fulfilled: The mean recovery was 78 % and RSDr did not exceed 8 %. The results of the SPE-HPLC online method were further compared to results obtained by liquid&–liquid extraction with stable isotope dilution analysis LC-MS/MS and found to be in good agreement. The developed SPE-HPLC online system with fluorescence detection allows a reliable, accurate, and sensitive quantification (limit of quantification, 30 µg/kg) of ZEN in edible oils while significantly reducing the workload. To our knowledge, this is the first report on an automated SPE-HPLC method based on a covalent SPE approach. KW - Dynamic covalent hydrazine chemistry (DCHC) KW - Maize germ oil KW - Food KW - Mycotoxin KW - ZEA KW - Isomerisation KW - Occurrence KW - Edible oil KW - SIDA KW - LC-MS/MS KW - Quantification PY - 2015 DO - https://doi.org/10.1007/s00216-015-8541-5 SN - 1618-2642 SN - 1618-2650 VL - 407 IS - 12 SP - 3489 EP - 3497 PB - Springer CY - Berlin AN - OPUS4-33067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholl, Juliane A1 - Lisec, Jan A1 - Haase, Hajo A1 - Koch, Matthias T1 - Identification of transformation products from fluorinated lithium-ion battery additives TPFPB and TPFPP: forever chemicals of tomorrow? N2 - AbstractFluorinated organic compounds (FOCs) represent a class of synthetic chemicals distinguished by their resilient carbon–fluorine bonds, which demonstrate an ability to withstand environmental degradation over an extended period. The integration of FOCs into cutting-edge applications, including lithium-ion batteries (LiBs), presents considerable potential for environmental harm that has not yet been sufficiently addressed. This study focuses on the environmental fate of two fluorinated aromatics, tris(pentafluorophenyl)borane (TPFPB) and tris(pentafluorophenyl)phosphine (TPFPP), given their important role in improving the performance of LiBs. To achieve this, laboratory simulation methods including total oxidizable precursor assay, electrochemistry (EC), Fenton reaction, UV-C irradiation, and hydrolysis were employed. Liquid chromatography and gas chromatography coupled with high-resolution mass spectrometry were used for identification of transformation products (TPs) and prediction of their molecular formulae. Despite the structural similarity between TPFPB and TPFPP, distinct differences in electrochemical behavior and degradation pathways were observed. TPFPB readily underwent hydroxylation and hydrolysis, resulting in a wide range of 49 TPs. A total of 28 TPs were newly identified, including oligomers and highly toxic dioxins. In contrast, TPFPP degraded exclusively under harsh conditions, requiring the development of innovative conditioning protocols for EC. In total, the simulation experiments yielded nine structurally different compounds, including seven previously undescribed, partially defluorinated TPs. This study highlights the potential risks associated with the use of FOCs in LiBs and provides insight into the complex environmental behavior of FOCs. KW - Mass Spectrometry KW - LiBs KW - POPs KW - Transformation products KW - Electrochemistry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611339 DO - https://doi.org/10.1007/s00216-024-05526-z SP - 1 EP - 15 PB - Springer Science and Business Media LLC AN - OPUS4-61133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maul, Ronald A1 - Müller, C. A1 - Rieß, Stephanie A1 - Koch, Matthias A1 - Methner, F.-J. A1 - Nehls, Irene T1 - Germination induces the glucosylation of the Fusarium mycotoxin deoxynivalenol in various grains N2 - In food, the mycotoxin deoxynivalenol (DON) often occurs in conjunction with its 3-β-D-glucopyranoside (D3G). The transformation of DON to D3G through glucosylation is catalysed by plant enzymes, however, the exact circumstances are not well understood. In order to investigate the role of enzymatic glucosylation in germinating grains, DON treated kernels were steeped and germinated under laboratory conditions. Furthermore, the effect of malting on the DON content of the contaminated barley was investigated. In all cases, DON and its derivatives were quantified by HPLC-MS/MS before, during and after the experiments. Amongst the six tested cereals; wheat, rye, barley, spelt, and millet transformed DON to D3G during germination whilst the oats were inactive. For wheat, barley, and spelt the initial DON content was reduced by 50%, with the loss being almost entirely accounted for by D3G formation. As D3G might be cleaved during digestion, the elevated D3G concentration may obscure the toxicologically relevant DON content in processed food and beer. The germination process has a major influence on the 'masking' of DON, leading to high quantities of D3G that may be missed in common mycotoxin analyses. KW - Mycotoxins KW - Masked mycotoxins KW - Deoxynivalenol (DON) KW - DON-3-glucoside KW - Acetyl-DON KW - Germination KW - Malting PY - 2012 DO - https://doi.org/10.1016/j.foodchem.2011.08.077 SN - 0308-8146 VL - 131 IS - 1 SP - 274 EP - 279 PB - Elsevier CY - Amsterdam [u.a.] ; Jena AN - OPUS4-25732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maul, Ronald A1 - Warth, B. A1 - Kant, Jill-Sandra A1 - Schebb, N.H. A1 - Krska, R. A1 - Koch, Matthias A1 - Sulyok, M. T1 - Investigation of the hepatic glucuronidation pattern of the fusarium mycotoxin deoxynivalenol in various species N2 - Deoxynivalenol (DON) is one of the most abundant mycotoxins contaminating food and feed worldwide. Upon absorption, the major portion of the toxin is excreted by humans and animal species as glucuronide. However, consistent in vitro data on DON glucuronidation are lacking. In the present study, the metabolism of DON was investigated using liver microsomes from humans and six different animal species. It was shown that all animal and human liver microsomes led to the formation of up to three different mono-O-glucuronides with significant interspecies differences. While the activity of human liver microsomes was low (0.8 to 2.2 pmol·min–1·mg–1), bovine liver and rat liver microsomes conjugated DON with activities of 525 pmol·min–1·mg–1 and 80 pmol·min–1·mg–1, respectively. KW - Deoxynivalenol KW - Hepatic metabolism KW - Microsomes KW - Glucuronidation KW - Inter-species comparison PY - 2012 DO - https://doi.org/10.1021/tx300348x SN - 0893-228X SN - 1520-5010 VL - 25 IS - 12 SP - 2715 EP - 2717 PB - Soc. CY - Washington, DC, USA AN - OPUS4-27604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholl, Juliane A1 - Meiers, Emelie A1 - Mauch, Tatjana A1 - Lisec, Jan A1 - Sommerfeld, Thomas A1 - Weinfurtner, Karlheinz A1 - Haase, Hajo A1 - Koch, Matthias T1 - Approaches towards sensitive and reliable determination of trifluoroacetic acid (TFA) from German grass- and farmland soils N2 - In light of the emerging threat of environmental contamination from per- and polyfluoroalkyl substances (PFAS), there is a growing need for analytical techniques that can be applied to a range of environmental matrices, including water, air, plant, and soil samples. Trifluoroacetic acid (TFA) is a member of the PFAS class, representing the shortest perfluorinated carboxylic acid and is an emerging pollutant whose environmental levels are expected to increase in the future. Soil matrices represent the interface between plant and ecosystem uptake of TFA, but contamination is poorly understood, largely due to a lack of uniform TFA determination methods. This study compares six ways of determining TFA in soils and highlights their limitations. We present a validated sample preparation method with high recoveries (104 %), low LOD (0.015 ng/g) and LOQ (0.045 ng/g). This approach includes isotope dilution analysis with hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry (HILIC-MS/MS) detection. The method was applied to quantify the TFA content in 100 soil samples from grassland and farmland across Germany. The results indicate the ubiquity of TFA, accompanied by elevated contamination levels in certain locations. An analysis of variance revealed no correlation with collection site and designation purpose. However, a low correlation was observed with dry bulk density. KW - PFAS KW - Extraction methods KW - HILIC-MS/M KW - Emerging pollutant KW - German soil protection PY - 2025 DO - https://doi.org/10.1016/j.chemosphere.2025.144496 SN - 0045-6535 VL - 382 SP - 1 EP - 11 PB - Elsevier CY - Amsterdam AN - OPUS4-63499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meiers, Emelie A1 - Scholl, Juliane A1 - Droas, Morten A1 - Vogel, Christian A1 - Leube, Peter A1 - Sommerfeld, Thomas A1 - Bagheri, A. A1 - Adam, Christian A1 - Seubert, A. A1 - Koch, Matthias T1 - Development and evaluation of analytical strategies for the monitoring of per- and polyfluoroalkyl substances from lithium-ion battery recycling materials N2 - Per- and polyfluoroalkyl substances (PFAS) are well-known as “forever chemicals” and persistent pollutants released by different anthropogenic sources. The potential release of PFAS from accumulating electronic waste and lithium-ion battery (LIB) recycling activities has gained increasing attention in the past years. This creates a need for analytical methods tailored for the determination of PFAS out of environmental matrices related to the named activities or directly out of the concerned materials. In this work, analytical strategies for the monitoring of PFAS in LIB recycling materials were explored for a group of legacy perfluoro sulfonic- and carbonic acids (PFSA and PFCA) and of fluorinated sulfonylimides suspected to be LIB electrolyte ingredients. These analytical strategies comprehend PFAS target approaches with a herein optimized liquid chromatography tandem mass spectrometry (LC–MS/MS) method equipped with a HILIC (hydrophilic interaction liquid chromatography) column in combination with the TOP (total oxidizable precursor) assay and an adapted sample preparation method for high-matrix LIB recycling materials. The validated target method was applied to a set of LIB recycling materials: end-of-life batteries, black masses from hydrometallurgical recycling, and gas absorption solutions from thermal treatment of black masses as part of the recycling procedure. Investigation results show that the LIB industry can be connected to the release of both “LIB”-PFAS, such as the target sulfonylimides, and “already-legacy” PFAS, like the PFSA and PFCA. Especially, the presence of trifluoroacetic acid (TFA) as an emerging pollutant in every investigated LIB material type underlines the threat of PFAS emissions from LIB waste and recycling activities. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Battery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647015 DO - https://doi.org/10.1007/s00216-025-06165-8 SN - 1618-2642 VL - 417 SP - 6567 EP - 6583 PB - Springer Science and Business Media LLC AN - OPUS4-64701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Scholl, Juliane A1 - Bagheri, Abbas A1 - Meiers, Emelie A1 - Lisec, Jan A1 - Russo, Francesco A1 - Haase, Hajo A1 - Koch, Matthias T1 - Unveiling Aging Mechanisms of Electrolytes in Commercial End-of-Life Lithium-Ion Batteries N2 - In this study, 77 end-of-life (EOL) commercial lithium-ion batteries (LIBs) of different formats were systematically analyzed to investigate electrolyte degradation mechanisms and the influence of pristine electrolyte composition on aging. Comprehensive chemical characterization employed targeted and non-targeted mass spectrometry (MS), combining liquid and gas chromatography (LC-MS/MS, GC-MS) with high-resolution MS (HRMS). This approach identified confirmed pristine components and complex degradation products. Commercial rechargeable pouch and cylindrical cells often deviated from conventional research model systems, using mixed lithium salt anions, ionic liquids (ILs), and high concentrations of triflates, triflimides, and bis(fluorosulfonyl)imide (FSI), functioning as solvents, salts, or additives. Specific IL degradation products and previously unreported pathways were proposed. A novel series of oligomerization products from propylene carbonate (PC) was also identified. In contrast, non-rechargeable coin cells showed prevalent use of per- and polyfluoroalkyl substances (PFAS) in their original electrolytes. Distinct PFAS degradation mechanisms were proposed for the first time. The absence of carbonate oligomers and lithium salt-derived products in coin cells, alongside standard carbonates, suggests lithium counterion coordination critically influences Lewis acid-catalyzed degradation. These findings provide new insight into real-world LIB aging, highlighting differences between commercial devices and model systems. KW - Mass Spectrometry KW - PFAS KW - Electrolyte degradation KW - Transformation products KW - Battery aging PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641059 DO - https://doi.org/10.2139/ssrn.5395937 SP - 1 EP - 15 PB - Elsevier BV AN - OPUS4-64105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholl, Juliane A1 - Lisec, Jan A1 - Bagheri, Abbas A1 - Meiers, Emelie A1 - Russo, Francesco Friedrich A1 - Haase, Hajo A1 - Koch, Matthias T1 - Unveiling aging mechanisms of electrolytes in commercial end-of-life lithium-ion batteries N2 - In this study, 77 end-of-life (EOL) commercial lithium-ion batteries (LIBs) of various formats were systematically analyzed to investigate electrolyte degradation and the influence of pristine electrolyte compositions on aging behavior. Comprehensive chemical characterization was conducted using targeted and non-targeted mass spectrometry (MS), employing LC-MS/MS, GC-MS, and high-resolution MS (HRMS). This integrated approach enabled the identification of confirmed pristine components and complex degradation products. The results show that rechargeable pouch and cylindrical cells often deviate from conventional model systems, containing mixed lithium salt anions, ionic liquids (ILs), and high concentrations of triflates, triflimides, and bis(fluorosulfonyl)imide (FSI). These function as solvents, salts, or safety-enhancing additives. Specific IL degradation products were identified, and hypotheses formulated on previously unreported pathways. Furthermore, a novel series of oligomerization products of propylene carbonate (PC) was detected. In contrast, non-rechargeable coin cells revealed widespread use of per- and polyfluoroalkyl substances (PFAS) in their original electrolytes. Based on ex situ analyses, hypothetical PFAS degradation mechanisms are proposed here for the first time. The absence of carbonate oligomers and lithium salt-derived products, alongside the presence of standard carbonates, indicates lithium counterion coordination as a key factor in Lewis acid-catalyzed degradation. This study offers valuable insights into real-world battery aging. KW - Transformation products KW - Lithium-ion batteries KW - Fluorinated Compounds KW - Gas chromatography/ QTOF-MS KW - HILIC-LC-MS/MS KW - PFAS KW - Electrochemistry PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644991 DO - https://doi.org/10.1016/j.jpowsour.2025.238613 SN - 0378-7753 VL - 661 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-64499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Recknagel, Sebastian A1 - Prinz, Carsten A1 - Vogel, Kristin A1 - Koch, Matthias A1 - Becker, Roland T1 - eCerto—versatile software for interlaboratory data evaluation and documentation during reference material production N2 - The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials. KW - Reference material KW - Statistics KW - Software KW - Collaborative trial PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591851 DO - https://doi.org/10.1007/s00216-023-05099-3 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-59185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Merkel, Stefan A1 - Dib, Baha A1 - Maul, Ronald A1 - Köppen, Robert A1 - Koch, Matthias A1 - Nehls, Irene T1 - Degradation and epimerization of ergot alkaloids after baking and in vitro digestion N2 - The degradation and epimerization of ergot alkaloids (EAs) in rye flour were investigated after baking cookies and subsequently subjecting them to an in vitro digestion model. Different steps of digestion were analyzed using salivary, gastric, and duodenal juices. The degradation and bidirectional conversion of the toxicologically relevant (R)-epimers and the biologically inactive (S)-epimers for seven pairs of EAs were determined by a HPLC method coupled with fluorescence detection. Baking cookies resulted in degradation of EAs (2–30 %) and a shift in the epimeric ratio toward the (S)-epimer for all EAs. The applied digestion model led to a selective toxification of ergotamine and ergosine, two ergotamine-type EAs. The initial percentage of the toxic (R)-epimer in relation to the total toxin content was considerably increased after digestion of cookies. Ergotamine and ergosine increased from 32 to 51 % and 35 to 55 %, respectively. In contrast, EAs of the ergotoxine type (ergocornine, α- and β-ergocryptine, and ergocristine) showed an epimeric shift toward their biologically inactive (S)-epimers. Further experiments indicated that the selective epimerization of ergotamine EAs occurs in the duodenal juice only. These results demonstrate that toxification of EAs in the intestinal tract should be taken into consideration. KW - HPLC-FLD KW - Claviceps purpurea KW - Rye KW - Ergotoxine KW - Ergotamine KW - Deoxynivalenol KW - Nivalenol KW - Zearalenone KW - Food KW - ERM KW - Quality assurance PY - 2012 DO - https://doi.org/10.1007/s00216-012-6386-8 SN - 1618-2642 SN - 1618-2650 VL - 404 IS - 8 SP - 2489 EP - 2497 PB - Springer CY - Berlin AN - OPUS4-27119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Merkel, Stefan A1 - Köppen, Robert A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Lumi-ergometrine - structural identification and occurrence in sclerotia N2 - The fungus Claviceps purpurea grows on grasses and cereal grains and produces six predominant ergot alkaloids. These toxic substances undergo different Transformation reactions during storage and cereal processing. One of these reactions is the addition of water to a double bond in the ergoline skeleton. Since light is required for this process, the substances formed were named lumi-ergot alkaloids. From these, a new asymmetric carbon and consequently two epimers with different polarities are formed. For investigations of lumi-ergot alkaloids, ergometrine was used exemplarily as it represents one of the six ergot Alkaloids predominantly formed by Claviceps purpurea. The main reaction product, the less polar compound of the two lumiergometrine epimers, was separated by HPLC and unambiguously identified as 10-(S)-lumi-ergometrine using X-ray structural analysis. A HPLC-MS/MS method was developed for the detection of this substance in sclerotia extracts. Using this method, the existence of both epimeric forms of lumiergometrinecould be proved in the sclerotia. This is the first time that the existence of a lumi-transformation product of ergot alkaloids was proved in naturally grown samples. KW - Lumi-ergot alkaloids KW - Sclerotia KW - Claviceps purpurea KW - HPLC-MS/MS PY - 2012 DO - https://doi.org/10.1007/s12550-011-0116-5 SN - 0178-7888 VL - 28 IS - 1 SP - 59 EP - 66 PB - Springer CY - Berlin; Heidelberg AN - OPUS4-25442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Bremser, Wolfram A1 - Stephan, Ina A1 - Klein-Hartwig, Karin A1 - Rasenko, Tatjana A1 - Koch, Matthias T1 - T-2 and HT-2 toxins in oat flakes: development of a certified reference material N2 - Trichothecene mycotoxins, with T-2 and HT-2 toxins being the main representatives of the type A subgroup, are naturally and worldwide occurring contaminants frequently found in grain-based food and feed. Due to the high consumption of these products and the potential health risk associated herewith, concerns about the safety and quality of food and feed have increased over the last decades at both governmental and consumer levels. Since it is not possible to avoid their occurrence, tremendous efforts have been performed to identify and monitor mycotoxins in food and feed to make their consumption safe. However, suitable certified reference materials (CRMs) intended for quality assurance and quality control purposes are still lacking for many mycotoxin-matrix combinations. Therefore, in the framework of a European Reference Material (ERM®) project, the first CRM for T-2 and HT-2 toxin in ground oat flakes (ERM®-BC720) was developed according to the requirements of ISO Guide 35. The whole process of ERM®-BC720 development, including sample preparation, homogeneity and stability studies and value assignment, is presented. The assignment of the certified mass fractions was based upon an in-house study using high-performance liquid chromatography isotope-dilution tandem mass spectrometry. Simultaneously, an interlaboratory comparison study involving 24 expert laboratories was conducted in order to support the in-house certification study. The certified values and their corresponding expanded uncertainties (k=2) for both T-2 and HT-2 toxin in ERM®-BC720, traceable to the international system of units, are (82±4) µg kg-1 and (81±4) µg kg-1, respectively. KW - Type A trichothecenes KW - Fusarium toxins KW - Isotope-dilution mass spectrometry KW - Food analysis KW - European Reference Material KW - Quality assurance PY - 2015 DO - https://doi.org/10.1007/s00216-014-8251-4 SN - 1618-2642 SN - 1618-2650 VL - 407 IS - 11 SP - 2997 EP - 3007 PB - Springer CY - Berlin AN - OPUS4-33073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schiro, G. A1 - Müller, T. A1 - Verch, G. A1 - Sommerfeld, Thomas A1 - Mauch, Tatjana A1 - Koch, Matthias A1 - Grimm, V. A1 - Müller, M.E.H. T1 - The distribution of mycotoxins in a heterogeneous wheat field in relation to microclimate, fungal and bacterial abundance N2 - Aim: To observe the variation in accumulation of Fusarium and Alternaria mycotoxins across a topographically heterogeneous field and tested biotic (fungal and bacterial abundance) and abiotic (microclimate) parameters as explanatory variables. Methods and Results: We selected a wheat field characterized by a diversified topography, to be responsible for variations in productivity and in canopy-driven microclimate. Fusarium and Alternaria mycotoxins where quantified in wheat ears at three sampling dates between flowering and harvest at 40 points. Tenuazonic acid (TeA), alternariol (AOH), alternariol monomethyl ether (AME), tentoxin (TEN), deoxynivalenol (DON), zearalenone (ZEN) and deoxynivalenol-3-Glucoside (DON.3G) were quantified. In canopy temperature, air and soil humidity were recorded for each point with data-loggers. Fusarium spp. as trichothecene producers, Alternaria spp. and fungal abundances were assessed using qPCR. Pseudomonas fluorescens bacteria were quantified with a culture based method. We only found DON, DON.3G, TeA and TEN to be ubiquitous across the whole field, while AME, AOH and ZEN were only occasionally detected. Fusarium was more abundant in spots with high soil humidity, while Alternaria in warmer and drier spots. Mycotoxins correlated differently to the observed explanatory variables: positive correlations between DON accumulation, tri 5 gene and Fusarium abundance were clearly detected. The correlations among the others observed variables, such as microclimatic conditions, varied among the sampling dates. The results of statistical model identification do not exclude that species coexistence could influence mycotoxin production. Conclusions: Fusarium and Alternaria mycotoxins accumulation varies heavily across the field and the sampling dates, providing the realism of landscapescale studies. Mycotoxin concentrations appear to be partially explained by biotic and abiotic variables. Significance and Impact of the Study: We provide a useful experimental design and useful data for understanding the dynamics of mycotoxin biosynthesis in wheat. KW - Alternaria KW - Deoxynivalenol KW - Food Safety KW - Fusarium KW - Pseudomonas fluorescens KW - Tenuazonic acid PY - 2019 DO - https://doi.org/10.1111/jam.14104 SN - 1365-2672 SN - 1364-5072 VL - 126 IS - 1 SP - 177 EP - 190 PB - Wiley AN - OPUS4-47161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471430 DO - https://doi.org/10.1088/0026-1394/56/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sebald, M.A. A1 - Gebauer, J. A1 - Sommerfeld, Thomas A1 - Koch, Matthias T1 - First Synthesis of (−)-Altenuene-D3 Suitable as Internal Standard for Isotope Dilution Mass Spectrometry N2 - Metabolites from Alternaria fungi exhibit a variety of biological properties such as phytotoxic, cytotoxic, or antimicrobial activity. Optimization of a literature procedure culminated in an efficient total synthesis of (−)-altenuene as well as a stable isotope-labeled derivative suitable for implementation in a LC-MS/MS method for mycotoxin analysis. KW - Altenuene KW - Alternaria mycotoxins KW - Food safety KW - Isotope-labeled KW - SIDA-LC-MS/MS KW - Suzuki coupling PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500696 DO - https://doi.org/10.3390/molecules24244563 SN - 1420-3049 VL - 24 SP - 4563 PB - MDPI CY - Basel AN - OPUS4-50069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Goren, A.C. A1 - Gokcen, T. A1 - Gunduz, S. A1 - Koch, Matthias A1 - Kaloulides, E. A1 - Giannikopoulou, P. A1 - Wai-Tong, G.T. A1 - Chan, A. T1 - Report on key comparison CCQM-K138: determination of aflatoxins (AFB(1), AFB(2), AFG(1), AFG(2) and total AFs) in dried fig N2 - The presence of any aflatoxin contamination in exported figs needs to be monitored and measured through reliable and traceable methods, which require pure and matrix certified reference materials. On the other hand, certified reference materials (CRM) for determination of aflatoxins in dried fig are not yet available. Moreover, there is a lack of CRMs to be used in routine testing laboratories for method validation and quality control. The routine testing laboratories, participating in commercial proficiency testing (PT) programs, use the results available from consensus values to evaluate the performance of the participating laboratories, rather than metrologically traceable assigned values. This study initially proposed as a key comparison and presented at the EURAMET TC-MC SCOA meeting in Malta in 2015 and subsequently at the CCQM OAWG meeting in April 2015, proposes a CRM candidate for determination of levels of aflatoxins B1, B2, G1, G2 and their total in dried. Evidence of successful participation in formal, relevant international comparisons are needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). In total nine NMI/DI participated in the Track C Key Comparison CCQM-K138 Determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and Total AFs) in Dried Fig. Participants were requested to evaluate the mass fractions expressed in ng/g units, of aflatoxins B1, B2, G1, G2 and total aflatoxin in a dried food matrix, dried fig. The CCQM-K138 results for the determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and total AFs) are ranging from 5.17 to 7.27 ng/g with an %RSD of 10.47 for AFB1, ranging from 0.60 to 0.871 ng/g with an %RSD of 11.69 for AFB2, ranging from 1.98 to 2.6 ng/g with an %RSD of 10.36 for AFG1, ranging from 0.06 to 0.32 ng/g with an %RSD of 35.6 for AFG2, and ranging from 8.29 to 10.31 ng/g with an %RSD of 7.69 for Total AFs. All participants based their analyses on LC-MS/MS, HPLC-FLD, HR-LC/MS, and IDMS. Brief descriptions of the analytical methods used by the participants, including sample preparation, analytical technique, calibrants, and quantification approach are summarized in Appendix F. Linear Pool was used to assign the Key Comparison Reference Values (KCRVs) for B1, B2, G1, G2 and total aflatoxins. Due to the traceability requirements for the calibrants not being met, results of KEBS, INTI, VNIIM and BAM were excluded from KCRV determination. Successful participation in CCQM-K138 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having high polarity (pKow > -2), in mass fraction range from 0.05 ng/g to 500 ng/g in dried food matrices. KW - Aflatoxins KW - Mycotoxins KW - Dried fig KW - Food contaminants PY - 2019 DO - https://doi.org/10.1088/0026-1394/56/1A/08008 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08008-1 EP - 08008-106 PB - IOP CY - Bristol AN - OPUS4-50326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mekonnen, Tessema Fenta A1 - Panne, Ulrich A1 - Koch, Matthias T1 - Glucosylation and Glutathione Conjugation of Chlorpyrifos and Fluopyram Metabolites Using Electrochemistry/Mass Spectrometry N2 - Xenobiotics and their reactive metabolites are conjugated with native biomolecules such as glutathione and glucoside during phase II metabolism. Toxic metabolites are usually detoxified during this step. On the other hand, these reactive species have a potential health impact by disrupting many enzymatic functions. Thus, it is crucial to understand phase II conjugation reactions of xenobiotics in order to address their fate and possible toxicity mechanisms. Additionally, conventional methods (in vivo and in vitro) have limitation due to matrix complexity and time-consuming. Hence, developing fast and matrix-free alternative method is highly demandable. In this work, oxidative phase I metabolites and reactive species of chlorpyrifos (insecticide) and fluopyram (fungicide) were electrochemically produced by using a boron-doped diamond electrode coupled online to electrospray mass spectrometry (ESI-MS). Reactive species of the substrates were trapped by biomolecules (glutathione and glucoside) and phase II conjugative metabolites were identified using liquid chromatography (LC)-MS/MS, and/or Triple time of flight (TripleTOF)-MS. Glutathione conjugates and glucosylation of chlorpyrifos, trichloropyridinol, oxon, and monohydroxyl fluopyram were identified successfully. Glutathione and glucoside were conjugated with chlorpyrifos, trichloropyridinol, and oxon by losing a neutral HCl. In the case of fluopyram, its monohydroxyl metabolite was actively conjugated with both glutathione and glucoside. In summary, seven bioconjugates of CPF and its metabolites and two bioconjugates of fluopyram metabolites were identified using electrochemistry (EC)/MS for the first time in this work. The work could be used as an alternative approach to identify glutathione and glucosylation conjugation reactions of other organic compounds too. It is important, especially to predict phase II conjugation within a short time and matrix-free environment. KW - Pesticide KW - Bioconjugation KW - Oxidative metabolism KW - EC/MS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475932 DO - https://doi.org/10.3390/molecules24050898 VL - 24 IS - 5 SP - 898 EP - 910 PB - MDPI AN - OPUS4-47593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Koch, Matthias A1 - Wise, S. A. A1 - Panne, Ulrich T1 - Fifteenth international symposium on biological and environmental reference materials (BERM-15) N2 - The 15th International Symposium on Biological and Environmental Reference Materials (BERM-15), organized by BAM, took place at in Berlin in September 2018. An overview on main topics of the conference is given. KW - BERM KW - Reference materials PY - 2019 DO - https://doi.org/10.1007/s00769-019-01377-9 SN - 1432-0517 SN - 0949-1775 VL - 24 IS - 3 SP - 249 EP - 250 PB - Springer Verlag AN - OPUS4-48203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Lisec, Jan A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - Prediction of transformation products of monensin by electrochemistry compared to microsomal assay and hydrolysis N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for animal health, food, and environmental matters. The active agent Monensin (MON) belongs to the ionophore antibiotics and is widely used as a veterinary drug against coccidiosis in broiler farming. However, no electrochemically (EC) generated TPs of MON have been described so far. In this study, the online coupling of EC and mass spectrometry (MS) was used for the generation of oxidative TPs. EC-conditions were optimized with respect to working electrode material, solvent, modifier, and potential polarity. Subsequent LC/HRMS (liquid chromatography/high resolution mass spectrometry) and MS/MS experiments were performed to identify the structures of derived TPs by a suspected target analysis. The obtained EC-results were compared to TPs observed in metabolism tests with microsomes and hydrolysis experiments of MON. Five previously undescribed TPs of MON were identified in our EC/MS based study and one TP, which was already known from literature and found by a microsomal assay, could be confirmed. Two and three further TPs were found as products in microsomal tests and following hydrolysis, respectively. We found decarboxylation, O-demethylation and acid-catalyzed ring-opening reactions to be the major mechanisms of MON transformation. KW - Transformation products KW - Monensin KW - Veterinary drugs KW - Electrochemistry KW - Hydrolysis KW - LC/HRMS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485689 DO - https://doi.org/10.3390/molecules24152732 SN - 1420-3049 VL - 24 IS - 15 SP - 2732, 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-48568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Keller, Julia A1 - Lörchner, Dominique A1 - Mekonnen, Tessema F. A1 - Koch, Matthias T1 - Transformation products of organic contaminants and residues - Overview of current simulation methods N2 - The formation of transformation products (TPs) from contaminants and residues is becoming an increasing focus of scientific community. All organic compounds can form different TPs, thus demonstrating the complexity and interdisciplinarity of this topic. The properties of TPs could stand in relation to the unchanged substance or be more harmful and persistent. To get important information about the generated TPs, methods are needed to simulate natural and manmade transformation processes. Current tools are based on metabolism studies, photochemical methods, electrochemical methods, and Fenton's reagent. Finally, most transformation processes are based on redox reactions. This review aims to compare these methods for structurally different compounds. The groups of pesticides, pharmaceuticals, brominated flame retardants, and mycotoxins were selected as important residues/contaminants relating to their worldwide occurrence and impact to health, food, and environmental safety issues. Thus, there is an increasing need for investigation of transformation processes and identification of TPs by fast and reliable methods. KW - Transformation product KW - Electrochemistry KW - Photochemistry KW - Fenton’s reagent PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474108 DO - https://doi.org/10.3390/molecules24040753 SN - 1420-3049 VL - 24 IS - 4 SP - 753, 1 EP - 23 PB - MDPI CY - Basel AN - OPUS4-47410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, Julia A1 - Borzekowski, Antje A1 - Koch, Matthias T1 - Mykotoxine in Lebensmitteln - Zearalenon und seine Transformationsprodukte N2 - Mykotoxine in Lebensmitteln stellen weltweit Probleme dar, Zearalenon in Speiseöl ist ein solches. Neue Hydrazinbasierte Analyseverfahren können jetzt helfen, den EU-Grenzwert besser zu kontrollieren. Aber auch die Strukturaufklärung von Transformationsprodukten und verlässliche Kalibrierstandards sind aktuelle Herausforderungen. KW - Analyseverfahren KW - Hydrazin KW - Speiseöle KW - Transformationsprodukte PY - 2019 IS - 03 SP - 34 EP - 36 AN - OPUS4-47858 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Borzekowski, Antje A1 - Anggriawan, R. A1 - Auliyati, M. A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. A1 - Karlovsky, P. A1 - Maul, Ronald T1 - Formation of Zearalenone Metabolites in Tempeh Fermentation N2 - Tempeh is a common food in Indonesia, produced by fungal fermentation of soybeans using Rhizopus sp., as well as Aspergillus oryzae, for inoculation. Analogously, for economic reasons, mixtures of maize and soybeans are used for the production of so-called tempeh-like products. For maize, a contamination with the mycoestrogen zearalenone (ZEN) has been frequently reported. ZEN is a mycotoxin which is known to be metabolized by Rhizopus and Aspergillus species. Consequently, this study focused on the ZEN transformation during tempeh fermentation. Five fungal strains of the genera Rhizopus and Aspergillus, isolated from fresh Indonesian tempeh and authentic Indonesian inocula, were utilized for tempeh manufacturing from a maize/soybean mixture (30:70) at laboratory-scale. Furthermore, comparable tempeh-like products obtained from Indonesian markets were analyzed. Results from the HPLC-MS/MS analyses show that ZEN is intensely transformed into its metabolites alpha-zearalenol (alpha-ZEL), ZEN-14-sulfate, alpha-ZEL-sulfate, ZEN-14-glucoside, and ZEN-16-glucoside in tempeh production. alpha-ZEL, being significantly more toxic than ZEN, was the main metabolite in most of the Rhizopus incubations, while in Aspergillus oryzae fermentations ZEN-14-sulfate was predominantly formed. Additionally, two of the 14 authentic samples were contaminated with ZEN, alpha-ZEL and ZEN-14-sulfate, and in two further samples, ZEN and alpha-ZEL, were determined. Consequently, tempeh fermentation of ZEN-contaminated maize/soybean mixture may lead to toxification of the food item by formation of the reductive ZEN metabolite, alpha-ZEL, under model as well as authentic conditions. KW - Modified mycotoxins KW - Zearalenone sulfate KW - a-zearalenol KW - Food fermentation KW - Rhizopus and Aspergillus oryzae PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491126 DO - https://doi.org/10.3390/molecules24152697 VL - 24 IS - 15 SP - 2697 PB - MDPI AN - OPUS4-49112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Temgoua, Ranil C. T. A1 - Lisec, Jan A1 - Koch, Matthias T1 - Breaking down phenylurea herbicides: advanced electrochemical approaches for environmental degradation and remediation N2 - Phenylurea herbicides (PUHs) represent one of the most extensively used herbicide families in agriculture worldwide. While effective for weed control, their environmental persistence, bioaccumulation potential, and formation of toxic metabolites raise significant environmental concerns. This review examines current electrochemical strategies for degrading phenylurea herbicides, with special emphasis on electrochemical oxidation (EC), photoelectrochemical processes (PEC), electro-Fenton (ECF) and photo-electro-Fenton (PECF), with particular attention to the various reactor configurations and their operational mechanisms. A critical innovation of this review lies in its systematic parameter assessment framework, which categorizes nine key operational parameters across all electrochemical degradation methods: electrode material, catalyst type, cell configuration, radiation source, operating conditions (pH, current density, temperature), removal efficiency, mineralization rate, degradation kinetics, identified intermediates, and Energy consumption. For each technique, we highlight which parameters are essential, important, critical, or non� applicable, providing a structured framework to guide future experimental design. Selected case studies are presented to illustrate practical applications and performance outcomes. The review concludes with acritical analysis of current knowledge gaps and future research avenues that could enhance the sustainability, efficiency, and scalability of electrochemical remediation technologies. This work is intended as a comprehensive resource for environmental chemists, analytical scientists, and remediation engineers committed to addressing phenylurea herbicide contamination. KW - Mass Spectrometry KW - Phenylurea herbicides KW - Electrochemistry PY - 2026 DO - https://doi.org/10.1039/D5EW00809C SN - 2053-1400 VL - 12 IS - 1 SP - 72 EP - 92 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andrae, K. A1 - Merkel, Stefan A1 - Durmaz, V. A1 - Fackeldey, K. A1 - Köppen, Robert A1 - Weber, M. A1 - Koch, Matthias T1 - Investigation of the ergopeptide epimerization process N2 - Ergopeptides, like ergocornine and a-ergocryptine, exist in an S- and in an R-configuration. Kinetic experiments imply that certain configurations are preferred depending on the solvent. The experimental methods are explained in this article. Furthermore, computational methods are used to understand this configurational preference. Standard quantum chemical methods can predict the favored configurations by using minimum energy calculations on the potential energy landscape. However, the explicit role of the solvent is not revealed by this type of methods. In order to better understand its influence, classical mechanical molecular simulations are applied. It appears from our research that 'folding' the ergopeptide molecules into an intermediate state (between the S- and the R-configuration) is mechanically hindered for the preferred configurations. KW - Ergopeptide KW - Epimerization KW - Hybrid monte carlo KW - Molecular dynamics KW - Conformation KW - Quantum mechanics PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-324632 DO - https://doi.org/10.3390/computation2030102 SN - 2079-3197 VL - 2 IS - 3 SP - 102 EP - 111 PB - MDPI CY - Basel AN - OPUS4-32463 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 - Merkel, Stefan A1 - Köppen, Robert A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Ergotaminine N2 - The title compound {systematic name: (6aR,9S)-N-[(2R,5S,10aS,10bS)-5-benzyl-10b-hydroxy-2-methyl-3,6-dioxooctahydro-8H-oxazolo[3,2-a]pyrrolo[2,1-c]pyrazin-2-yl]-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide}, C33H35N5O5, was formed by an epimerization reaction of ergotamine. The non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar [maximum deviation = 0.317 (4) Å] and shows an envelope conformation, whereas ring D, involved in an intramolecular N–H···N hydrogen bond exhibits a slightly distorted chair conformation. The structure displays chains running approximately parallel to the diagonal of bc plane that are formed through N–H···O hydrogen bonds. PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-254528 DO - https://doi.org/10.1107/S1600536812003674 SN - 1600-5368 VL - 68 IS - 3 SP - o610-o611, sup1-sup11 PB - Munksgaard CY - Copenhagen AN - OPUS4-25452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Merkel, Stefan A1 - Köppen, Robert A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Lysergol monohydrate N2 - In the title compound [systematic name: (7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3,2-fg]quinoline-9-yl)methanol monohydrate], C16H18N2O·H2O, the non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar, with a maximum deviation of 0.659 (3) Å, and shows an envelope conformation. In the crystal, hydrogen bonds between the lysergol and water molecules contribute to the formation of layers parallel to (10-2). PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-254015 DO - https://doi.org/10.1107/S1600536812002632 SN - 1600-5368 VL - 68 IS - 2 SP - o523, sup1 EP - sup8 PB - Munksgaard CY - Copenhagen AN - OPUS4-25401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Meermann, Björn A1 - Koch, Matthias A1 - Weller, Michael G. T1 - Editorial: Analytical methods and applications in materials and life sciences N2 - Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials. This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences. However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences. The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - Analysis KW - Life sciences KW - Analytical sciences KW - Quality assurance KW - Reference material KW - Fluorescence KW - Nanoparticle KW - Sensor KW - Material sciences KW - Pollutant KW - Environment KW - Method KW - Limit of detection KW - 150th anniversary KW - ABC KW - BAM KW - Collection KW - Editorial KW - Special issue KW - Bundesanstalt für Materialforschung und -prüfung KW - Jahrestag PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550720 DO - https://doi.org/10.1007/s00216-022-04082-8 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - Topical collection: Analytical methods and applications in the materials and life sciences SP - 4267 EP - 4268 PB - Springer CY - Berlin AN - OPUS4-55072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghiringhelli, Luca M. A1 - Baldauf, Carsten A1 - Bereau, Tristan A1 - Brockhauser, Sandor A1 - Carbogno, Christian A1 - Chamanara, Javad A1 - Cozzini, Stefano A1 - Curtarolo, Stefano A1 - Draxl, Claudia A1 - Dwaraknath, Shyam A1 - Fekete, Ádám A1 - Kermode, James A1 - Koch, Christoph T. A1 - Kühbach, Markus A1 - Ladines, Alvin Noe A1 - Lambrix, Patrick A1 - Himmer, Maja-Olivia A1 - Levchenko, Sergey V. A1 - Oliveira, Micael A1 - Michalchuk, Adam A1 - Miller, Ronald E. A1 - Onat, Berk A1 - Pavone, Pasquale A1 - Pizzi, Giovanni A1 - Regler, Benjamin A1 - Rignanese, Gian-Marco A1 - Schaarschmidt, Jörg A1 - Scheidgen, Markus A1 - Schneidewind, Astrid A1 - Sheveleva, Tatyana A1 - Su, Chuanxun A1 - Usvyat, Denis A1 - Valsson, Omar A1 - Wöll, Christof A1 - Scheffler, Matthias T1 - Shared metadata for data-centric materials science N2 - The expansive production of data in materials science, their widespread sharing and repurposing requires educated support and stewardship. In order to ensure that this need helps rather than hinders scientific work, the implementation of the FAIR-data principles (Findable, Accessible, Interoperable, and Reusable) must not be too narrow. Besides, the wider materials-science community ought to agree on the strategies to tackle the challenges that are specific to its data, both from computations and experiments. In this paper, we present the result of the discussions held at the workshop on “Shared Metadata and Data Formats for Big-Data Driven Materials Science”. We start from an operative definition of metadata, and the features that a FAIR-compliant metadata schema should have. We will mainly focus on computational materials-science data and propose a constructive approach for the FAIRification of the (meta)data related to ground-state and excited-states calculations, potential-energy sampling, and generalized workflows. Finally, challenges with the FAIRification of experimental (meta)data and materials-science ontologies are presented together with an outlook of how to meet them. KW - Library and Information Sciences KW - Statistics, Probability and Uncertainty KW - Computer Science Applications KW - Education KW - Information Systems KW - Statistics and Probability PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584846 DO - https://doi.org/10.1038/s41597-023-02501-8 VL - 10 IS - 1 SP - 1 EP - 18 PB - Springer Science and Business Media LLC AN - OPUS4-58484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drzymala, Sarah A1 - Kraus, Werner A1 - Emmerling, Franziska A1 - Koch, Matthias T1 - (3S)-14,16-Dihydroxy-3-methyl-3,4,5,6,9,10,11,12-octa-hydro-1H-2-benzoxacyclotetradecine-1,7(8H)-dione (zearalanone) monohydrate N2 - The absolute configuration of the title compound, C18H24O5·H2O, was not been determined by anomalous-dispersion effects, but has been assigned by reference to an unchanging chiral centre in the synthetic procedure. Intramolecular O—H···O hydrogen bonds stabilize the molecular conformation. In the crystal, O—H···O hydrogen bonds link the main molecules and the water molecules, forming an infinite three-dimensional network. KW - Zearalanone KW - Crystal structure PY - 2012 DO - https://doi.org/10.1107/S1600536812018168 SN - 1600-5368 VL - 68 IS - 5 SP - o1577, sup1 EP - sup7 PB - Munksgaard CY - Copenhagen AN - OPUS4-25832 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -