TY - JOUR A1 - Gärtner, Sonja A1 - Balski, Matthias A1 - Koch, Matthias A1 - Nehls, Irene T1 - Analysis and migration of phthalates in infant food packed in recycled paperboard N2 - The contamination of infant food with substances from its packaging due to migration processes is still a problem. Most recently, great attention was paid to the migration of epoxidized soybean oil (ESBO) and phthalates from twist-off closures into baby food packed in glass jars. Besides, packaging made of recycled fiber materials such as paper and paperboard were found to be the source of contaminants in dry and powdery foodstuffs such as sugar, rice, and maize flour. In this study 20 infant food samples packed in recycled paperboard containers were tested for phthalates and diisopropyl naphthalenes (DIPN), known incorporated substances in recycled paper. Furthermore, the barrier function of different secondary packaging materials (paper and aluminum-coated foil) was investigated. The highest contents of phthalates (mainly diisobutyl phthalate, DiBP) and DIPN in infant food samples were found for those foods packed in inner bags made of paper. Migration experiments were performed under authentic conditions to evaluate possible transfer mechanism (gas phase, direct contact) of phthalate esters into foodstuff. It is shown that paper does not provide an appropriate barrier against migration of semipolar compounds such as phthalates. The air space itself otherwise effectively prevents migration of the less volatile phthalates under the applied conditions. KW - Phthalates KW - Accelerated solvent extraction (ASE) KW - Infant food KW - Recycled paper KW - Migration KW - GC-MS PY - 2009 U6 - https://doi.org/10.1021/jf902683m SN - 0021-8561 SN - 1520-5118 VL - 57 IS - 22 SP - 10675 EP - 10681 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-20472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siegel, David A1 - Andrae, K. A1 - Proske, Matthias A1 - Kochan, Cindy A1 - Koch, Matthias A1 - Weber, M. A1 - Nehls, Irene T1 - Dynamic covalent hydrazine chemistry as a selective extraction and cleanup technique for the quantification of the Fusarium mycotoxin zearalenone in edible oils N2 - A novel, cost-efficient method for the analytical extraction of the Fusarium mycotoxin zearalenone (ZON) from edible oils by dynamic covalent hydrazine chemistry (DCHC) was developed and validated for its application with high performance liquid chromatography-fluorescence detection (HPLC-FLD). ZON is extracted from the edible oil by hydrazone formation on a polymer resin functionalised with hydrazine groups and subsequently released by hydrolysis. Specifity and precision of this approach are superior to liquid partitioning or gel permeation chromatography (GPC). DCHC also extracts zearalanone (ZAN) but not α-/β-zearalenol or -zearalanol. The hydrodynamic properties of ZON, which were estimated using molecular simulation data, indicate that the compound is unaffected by nanofiltration through the resin pores and thus selectively extracted. The method's levels of detection and quantification are 10 and 30 µg/kg, using 0.2 g of sample. Linearity is given in the range of 10-20,000 µg/kg, the average recovery being 89%. Bias and relative standard deviations do not exceed 7%. In a sample survey of 44 commercial edible oils based on various agricultural commodities (maize, olives, nuts, seeds, etc.) ZON was detected in four maize oil samples, the average content in the positive samples being 99 µg/kg. The HPLC-FLD results were confirmed by HPLC-tandem mass spectrometry and compared to those obtained by a liquid partitioning based sample preparation procedure. KW - Zearalenone KW - Extraction KW - Edible oil KW - Maize KW - Dynamic covalent hydrazine chemistry KW - Hydrazone KW - SPE KW - Hydrodynamic radius KW - HPLC-FLD PY - 2010 U6 - https://doi.org/10.1016/j.chroma.2010.02.019 SN - 0021-9673 VL - 1217 IS - 15 SP - 2206 EP - 2215 PB - Elsevier CY - Amsterdam AN - OPUS4-21048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, M.E.H. A1 - Steier, I. A1 - Köppen, Robert A1 - Proske, Matthias A1 - Korn, U. A1 - Koch, Matthias A1 - Siegel, David T1 - Cocultivation of phytopathogenic Fusarium and Alternaria strains affects fungal growth and mycotoxin production N2 - Aims: A laboratory study was conducted to evaluate the influence of cocultivation of toxigenic Fusarium (F.) and Alternaria (A.) fungi with respect to growth and mycotoxin production. Methods and Results: Fusarium culmorum Fc13, Fusarium graminearum Fg23 and two Alternaria tenuissima isolates (At18 and At220) were simultaneously or consecutively co-incubated on wheat kernels in an in vitro test system. Fungal biomass was quantified by determining ergosterol content. Three Fusarium toxins (DON, NIV and ZON) and three Alternaria toxins (AOH, AME and ALT) were analysed by a newly developed HPLC/MS/MS method. In simultaneous cocultures, the fungal biomass was enhanced up to 460% compared with individual cultures; Alternaria toxins were considerably depressed down to <5%. Combining At18 and At220 with Fg23 inhibited the toxin production of both fungal partners. In contrast, Fc13 increased its DON and ZON production in competitive interaction with both A. strains. Conclusions: The interfungal competitive effects aid the understanding of the processes of competition of both fungi in natural environments and the involvement of mycotoxins as antifungal factors. Significance and Impact of Study: Cocultivation significantly affects fungal growth and mycotoxin production of phytopathogenic Alternaria and Fusarium strains. The impact of mycotoxins on the interfungal competition is highlighted. KW - Alternaria KW - Cocultivation KW - Ergosterol KW - Fusarium KW - Interfungal competition KW - Multimycotoxin analysis PY - 2012 U6 - https://doi.org/10.1111/j.1365-2672.2012.05388.x SN - 1364-5072 VL - 113 IS - 4 SP - 874 EP - 887 PB - Wiley-Blackwell CY - Malden, Mass., USA AN - OPUS4-26932 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Riedel, Juliane A1 - Proske, Matthias A1 - Drzymala, Sarah A1 - Rasenko, Tatjana A1 - Durmaz, V. A1 - Weber, M. A1 - Koch, Matthias T1 - Photochemical trans-/cis-isomerization and quantitation of zearalenone in edible oils N2 - The emphasis of the present work was to investigate the photochemical conversion of trans- to cis-zearalenone in edible oils under real-life conditions. For quantitation purposes a cis-zearalenone standard was synthesized and characterized for its identity and purity (≥95%) by 1H NMR, X-ray crystallography, HPLC fluorescence and mass spectrometric detection. In a sample survey of 12 edible oils (9 corn oils, 3 hempseed oils) from local supermarkets all corn oils contained trans-zearalenone (median 194 µg/kg), but no cis-zearalenone was detected. For alteration studies trans-zearalenone contaminated corn oils were exposed to sunlight over 4 and 30 weeks, revealing an obvious shift toward cis-zearalenone up to a cis/trans ratio of 9:1 by storage in colorless glass bottles. Irradiation experiments of trans-zearalenone in different organic solvents confirmed the preferred formation of cis-zearalenone possibly caused by entropic effects rather than by enthalpic entities as investigated by quantum chemical and classical force field simulations. KW - Fusarium mycotoxins KW - Food KW - Analysis KW - Occurrence PY - 2012 U6 - https://doi.org/10.1021/jf3037775 SN - 0021-8561 SN - 1520-5118 VL - 60 IS - 47 SP - 11733 EP - 11740 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-27375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Recknagel, Christoph A1 - Eichler, Antje A1 - Koch, Matthias A1 - Proske, Matthias A1 - Huth, Christian T1 - Reflexkörper und Griffigkeitsmittel in Nachstreumittelgemischen für Markierungssysteme - Entwicklung von Prüfmethoden zur Separation sowie Analyse und Identifikation der Beschichtung (Coating/Treatment) von Reflexkörpern KW - Sicherheit der Verkehrsinfrastruktur KW - Fahrbahnmarkierungen PY - 2014 SN - 978-3-95606-061-8 SN - 0943-9331 IS - V 232 SP - 1 EP - 166 PB - Fachverlag NW in der Carl Schünemann Verlag GmbH CY - Bergisch Gladbach AN - OPUS4-30386 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siegel, David A1 - Feist, M. A1 - Proske, Matthias A1 - Koch, Matthias A1 - Nehls, Irene T1 - Degradation of the alternaria mycotoxins alternariol, alternariol monomethyl ether, and altenuene upon bread baking N2 - The stability of the Alternaria mycotoxins alternariol, alternariol monomethyl ether, and altenuene upon bread baking was investigated by model experiments using a spiked wholemeal wheat flour matrix. For alternariol and alternariol monomethyl ether, but not for altenuene, degradation products, formed through a sequence of hydrolysis and decarboxylation, could be identified in pilot studies. The simultaneous quantification of alternariol, alternariol monomethyl ether, altenuene, and the degradation products was achieved by a newly developed high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) multimethod. The obtained quantitative data indicate that the Alternaria mycotoxins are barely degraded during wet baking, while significant degradation occurs upon dry baking, with the stability decreasing in the order alternariol monomethyl ether > alternariol > altenuene. The novel degradation products could be detected after the wet baking of flour spiked with alternariol and in a sample survey of 24 commercial cereal based baking products. KW - Alternariol monomethyl ether KW - Alternariol KW - Altenuene KW - Degradation KW - Baking KW - Bread KW - HPLC-MS/MS PY - 2010 U6 - https://doi.org/10.1021/jf102156w SN - 0021-8561 SN - 1520-5118 VL - 58 IS - 17 SP - 9622 EP - 9630 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-21909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Gärtner, Sonja A1 - Balski, Matthias A1 - Köppen, Robert A1 - Nehls, Irene T1 - Aus der Kartonverpackung in die Babynahrung N2 - Lebensmittel in Recyclingkartons finden sich längst in allen Supermärkten. Doch die schützende Verpackung kann zu einer Quelle für Kontaminationen durch Phthalate werden. Analytik und Migration dieser hormonell wirksamen Weichmacher sind daher ein aktueller Forschungsschwerpunkt. KW - Analytische Chemie KW - Lebensmittelchemie KW - Umweltanalytik KW - Gaschromatographie KW - Massenspektrometrie PY - 2011 U6 - https://doi.org/10.1002/nadc.201178449 SN - 1439-9598 SN - 1521-3854 VL - 59 IS - 5 SP - 544 EP - 546 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-23639 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwake-Anduschus, C. A1 - Proske, Matthias A1 - Sciurba, E. A1 - Muenzing, K. A1 - Koch, Matthias A1 - Maul, Ronald T1 - Distribution of deoxynivalenol, zearalenone, and their respective modified analogues in milling fractions of naturally contaminated wheat grains N2 - Mycotoxins are among the most abundant contaminants in food and feed worldwide. Therefore, in the EU maximum levels are established, e.g. for the frequently occurring Fusarium toxins deoxynivalenol (DON) and zearalenone (ZEA). Additional to DON and ZEA, modified mycotoxins are present in naturally contaminated grain products contributing significantly to the exposure of humans and animals with mycotoxins. Up to now data on the spatial distribution of many (masked) mycotoxins in the kernels of wheat are missing. The aim of the present study was to investigate the amounts of DON and ZEA as well as their most abundant derivatives DON-3-glucoside (DON-3G), 3- and 15-acetyl-DON, ZEA-14- and 16-glucoside and ZEA-14-sulphate (ZEA-14S) in mill fractions of naturally contaminated wheat batches using HPLC-MS/MS. The investigated distribution pattern in ten milling fractions is comparable among the three investigated different wheat batches. Interestingly, DON and DON-3G were found to be present to similar amounts in all fractions. In bran, the levels were only slightly higher than in the endosperm. By contrast, for ZEA and ZEA-14S a significantly higher amount of toxin is located in the fibre-rich fractions. The relative mass proportion of DON-3G comprises for only between 2.9 and 11.2% of the free DON, while the relative mass proportion of ZEA-14S is estimated to even exceed the amount of free ZEA in certain fractions. Acetylated DON derivatives and ZEA-glucosides were only detected in low amounts. The experimental results show that a significant reduction of the ZEA and ZEA-14S level in wheat flour is feasible by applying milling technology strategies. However, the almost evenly distribution of DON and DON-3G in all fractions does not allow for the technological removal of relevant toxin amounts. Furthermore, the relative share of masked forms was higher for ZEA derivatives than for the DON conjugates in the investigated wheat lots. KW - Mass spectrometry KW - Fusarium mycotoxins KW - Masked mycotoxin KW - Flour extraction KW - Bran PY - 2015 U6 - https://doi.org/10.3920/WMJ2014.1818 SN - 1875-0710 SN - 1875-0796 VL - 8 IS - 4 SP - 433 EP - 443 PB - Wageningen Academic Publishers CY - Wageningen AN - OPUS4-33833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Matthias A1 - Liebich, Almuth A1 - Win, Tin A1 - Nehls, Irene T1 - Certified Reference Materials for the determination of mineral oil hydrocarbons in water, soil and waste N2 - The international research project HYCREF, funded by the European Commission in the 5 th Framework programme, aimed to develop methods to prepare homogenous and stable water-, soiland waste reference materials contaminated with mineral oil hydrocarbons and to test certify the mineral oil content by gas chromatographic methods. As mineral oil products are important sources for environmental contaminations a high need exists for certified reference materials for their determination using the new gas chromatographic methods (soil: ISO/FDIS 16703, waste: ENpr 14039, water: ISO 9377-2). The experimental conditions and results for preparation and characterisation of a total of nine reference materials (3 water-, 3 soil- and 3 waste materials) are described and discussed. Target values for the reference materials were defined at the beginning of the project in order to have clear quality criteria, which could be compared with the achieved results at the end of the project. These target specifications were related to the maximum uncertainty from test certification exercises (< 5 % for soil/waste and < 10 % for water), the maximum inhomogeneity between bottles (< 3 %) and minimum requirements for stability (> 5 years for soil/waste and > 2 years for water). The feasibility studies showed that solid materials (soil, waste) could be prepared sufficiently homogenous and stable. The test certified values of the 6 solid materials comprise a wide range of mineral oil content from about 200-9000 mg/kg with expanded uncertainties between 5.7-13.1 % using a coverage factor k (k = 2). The development of new water reference materials –the so-called “spiking pills” for an offshore- and a land-based discharge water represents one of the most innovative aspects of the project. The spiking pill technology facilitates the application and storage and improves the material stability compared with aqueous materials. Additional to the preparation and test certification of the reference materials investigations on the analytical method for the determination of mineral oil hydrocarbons were performed. The results obtained in relation to the optimisation of analytical method (extraction procedure, sample pretreatment, clean-up and measurement) were provided to the respective working group of ISO/TC 190, ISO/TC 147 and CEN/TC 292 and were incorporated into the ongoing standardisation procedures. The new version of ISO/FDIS 16703 (July 2004) includes the improvements based on HYCREF results, for example the increase of the solvent/sample ratio, the removal of acetone from the organic extracts and the use of column technique instead of batch technique for clean-up. T3 - BAM Forschungsberichtreihe - 272 PY - 2005 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-1795 SN - 978-3-86509-363-9 SN - 0938-5533 VL - 272 SP - 1 EP - 92 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Becker, Roland A1 - Koch, Matthias A1 - Buge, Hans-Georg A1 - Nehls, Irene T1 - Entwicklung eines Referenzverfahrens zur Quantifizierung von polychlorierten Biphenylen (PCB) in Kunststoffgranulaten N2 - Im Rahmen eines vom Bundesministerium für Wirtschaft und Arbeit (BMWA) geförderten Projektes wird in Kooperation mit dem Verband deutscher Metallhändler (VDM) ein Verfahren zur Quantifizierung der PCB-Kongenere 28, 52, 101, 138, 153, 180 im Gehaltsbereich von 0,1 bis 20 mg in Kunststoffabfällen aus dem Altkabelrecycling entwickelt und validiert. Dazu werden repräsentative Referenzmaterialien für die Laboranalytik aus Granulaten verschiedener Kabelzerlegeprozesse hergestellt und charakterisiert. Die Methodenentwicklung umfasst mahl-, sieb- und schüttguttechnologische Aspekte sowie den Vergleich unterschiedlicher Extraktionsverfahren und chromatographischer Bedingungen. Das validierte Verfahren sieht die Mahlung der technischen Probe auf eine Kornobergrenze von 0,50 mm gefolgt von Extraktion mit einem unpolaren Lösungsmittel bei einer Einwaage von 4 g und gaschromatographischer Bestimmung vor. Die Bestimmungsgrenzen liegen zwischen 0,01 und 0,08 mg/kg. Bei sorgfältiger Wahl der chromatographischen Bedingungen sind Elektroneneinfang- und massenselektive Detektion (MS) gleichwertig. In Gegenwart größerer Mengen bestimmter Komponenten, die in einigen Kabeln enthalten sind, kann der Einsatz eines MS von Vorteil sein. Drei Referenzmaterialien mit Gehalten der genannten Kongenere zwischen 0,1 bis 5 mg/kg werden in einem abschließenden Ringversuch zur Validierung dieser Methode mit 23 ausgewählten Laboratorien eingesetzt. Dabei ergeben sich für die Quantifizierung dieser Kongenere relative Vergleichsstandardabweichungen zwischen 15 und 33 %. Das Verfahren wird in die europäische Normung (CEN 292 „Characterisation of Waste“) eingebracht. T3 - BAM Forschungsberichtreihe - 270 PY - 2005 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-1810 SN - 978-3-86509-320-5 SN - 0938-5533 VL - 270 SP - 1 EP - 107 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-181 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -