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 - Koch, Matthias A1 - Labsch, Erika A1 - Köppen, Robert A1 - Witt, Angelika A1 - Nehls, Irene T1 - Feuchtebestimmung in Lebensmitteln durch coulometrische Karl-Fischer-Titration nach thermischer Wasserfreisetzung KW - KFT KW - Wassergehalt KW - Standardaddition PY - 2010 SN - 0012-0413 SN - 1869-2214 VL - 106 IS - Mai SP - 251 EP - 254 PB - Wiss. Verl.-Ges. CY - Stuttgart AN - OPUS4-21351 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Liebich, Almuth A1 - Win, Tin A1 - Nehls, Irene A1 - Kvernheim, A.L. A1 - Ringstad, O. A1 - Oreld, F. T1 - Feasibility studies for the preparation and certification of reference materials - Part II: Mineral oil contaminated waste materials N2 - The 2-year international joint project HYCREF (Contract-No. G6RD-CT-2002-00854), funded by the European Commission in the 5th Framework programme, aimed to develop methods to prepare homogenous and stable water-, soil- and 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, appropriate reference materials certified by using the new gas chromatographic methods (soil: ISO/FDIS 16703, waste: prEN 14039 and KW/04, water: ISO 9377-2) are highly needed. Additional to the HYCREF-results presented in part I–mineral contaminated soils–this second paper gives an overview of the feasibility study for the preparation and test certification of three waste reference materials (offshore marine sediment, building material and industrial waste). The following specifications, which had been defined in the project work plan, were reached successfully: uncertainty of the mineral oil content resulting from the certification exercise ≤ 5% and a between-bottle inhomogeneity of ≤ 3%. All three materials have been evaluated for long- and short term stability. They contain different levels and types of mineral oil and cover the full application range of ISO/FDIS 16703 and prEN 14039 (100–10,000 mg/kg). The expanded uncertainties U cert of the three materials are about 6%. In this way, they are comparable to ERM®-CC015a (U cert=7.1%, mineral oil in a river sediment) and are suited to close the present gap of commercially available CRM for mineral oil determination in waste. KW - Mineral oil hydrocarbons KW - Feasibility study KW - Certified reference materials (CRM) KW - Waste materials KW - Gas chromatography PY - 2006 SN - 0949-1775 SN - 1432-0517 VL - 11 IS - 3 SP - 122 EP - 129 PB - Springer CY - Berlin AN - OPUS4-12392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Win, Tin T1 - Feasibility and limits in preparation of reference materials for the organic emvironmental analysis T2 - EUROENVIRONMENT II CY - Vienna, Austria DA - 1995-10-18 PY - 1995 AN - OPUS4-5659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Win, Tin A1 - Erhardt, Ulla T1 - Externe Qualitätssicherung im Grundwassermonitoring T2 - Weiterbildungsveranstaltung der Mitarbeiter der Umweltämter; Verwaltungsakademie Berlin CY - Berlin, Germany DA - 2004-03-02 PY - 2004 AN - OPUS4-6943 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Johnen, D. A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Fischer-Tenhagen, C. T1 - Evaluierung der Fähigkeit zur Geruchsgeneralisierung und Differenzierung von Hunden im Modellversuch T2 - Symposium Odorologie CY - Hamburg DA - 2015-03-23 PY - 2015 AN - OPUS4-32831 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Philipp, Rosemarie A1 - Hanebeck, Olaf A1 - Hein, Sebastian A1 - Bremser, Wolfram A1 - Win, Tin A1 - Nehls, Irene T1 - Ethanol/water solutions as certified reference materials for breath alcohol analyzer calibration N2 - The Federal Institute for Materials Research and Testing (BAM), Germany, has issued a series of large volume ethanol in water certified reference materials (CRMs), primarily developed for the calibration of evidential breath alcohol analyzers in Germany. The certified parameter is the ethanol mass concentration at 20 °C. When used in a wet bath simulator, the solutions deliver gas samples that meet the requirements set by the Organization of Legal Metrology for calibration of breathalyzers. The materials were prepared gravimetrically by spiking of ethanol into water in single 5 L units. A complete uncertainty budget for the preparation process has been established. The purity of the commercial ethanol stock solution was identified to be the main source of uncertainty. For stability and homogeneity measurements and for the verification of the gravimetric mass concentration of the CRMs, a robust high-precision gas chromatography, with flame-ionization detection method for ethanol determination in aqueous samples was developed and validated. The good performance of this method has been demonstrated in several international comparisons organized by the Consultative Committee for Amount of Substance-Metrology in Chemistry at the International Bureau of Weights and Measures. KW - Certified reference material KW - Ethanol in water KW - Breath alcohol KW - GC-FID PY - 2010 DO - https://doi.org/10.1007/s00769-009-0605-9 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 3 SP - 141 EP - 146 PB - Springer CY - Berlin AN - OPUS4-20999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Mönch, Bettina A1 - Jung, Christian A1 - Becker, Roland T1 - EtG in Haaren - Biomarker für den Alkoholkonsum T2 - Multiparameteranalytik, Innovationsforum CY - Senftenberg, Germany DA - 2012-03-16 PY - 2012 AN - OPUS4-25663 LA - deu 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 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 - Ergometrinine N2 - The absolute configuration of ergometrinine, C19H23N3O2 {systematic name: (6aR,9S)-N-[(S)-1-hydroxypropan-2-yl]-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide}, was established based on epimerization reaction of ergometrine, which was followed by preparative HPLC. The non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar [maximum deviation = 0.271 (3) Å] and shows an envelope conformation, whereas ring D, involved in an intramolecular N-HN hydrogen bond, exibits a slightly distorted chair conformation. The structure displays undulating layers in the ac plane formed by O-H...O and N-H...O hydrogen bonds. KW - Ergometrinine KW - Ergometrine KW - Ergot alkaloids KW - Indole alkaloids KW - Crystal structure KW - Epimerization PY - 2010 DO - https://doi.org/10.1107/S1600536810030825 SN - 1600-5368 VL - 66 IS - 9 SP - o2275, sup-1 - sup-9 PB - Munksgaard CY - Copenhagen AN - OPUS4-21806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Win, Tin A1 - Schmieder, Rosemarie A1 - Erhardt, Ulla A1 - Walther, Wolfgang A1 - Buge, Hans-Georg A1 - Nehls, Irene A1 - Tzscheutschler, Erika T1 - Erarbeitung und Validierung eines standardisierbaren Analysenverfahrens für die Bestimmung von LHKW und BTEX in Boden, Bereitstellung eines Referenzmaterials und Überprüfung des Verfahrens in einem Ringversuch N2 - Ziel des Vorhabens war die Erarbeitung und Validierung eines standardisierbaren Analysenverfahrens für die Bestimmung von leichtflüchtigen Halogenkohlenwasserstoffen (LHKW) und monoaromatischen Verbindungen wie Benzol, Toluol, Ethylbenzol und Xylolen (BTEX) in Boden, die Bereitstellung eines geeigneten Boden-Referenzmaterials dafür und die Durchführung eines Validierungsringversuches. Da die leichtflüchtigen Verbindungen in dem von den kontaminierten Standorten angeschafften Boden schon während des Verarbeitungsprozesses weitgehend verloren gegangen waren, wurde das LHKW- und BTEX-haltige Referenzmaterial durch Einzelflaschendotierung hergestellt. Eine bestimmte Menge eines im Rahmen eines vorhergehenden BMBF-Vorhabens (Förderkennzeichen 07 OTX 20/3) erhaltenen unbelasteten Ackerboden-Referenzmaterials wurde in Glasflaschen eingewogen und unter optimierten Bedingungen mit einer methanolischen Lösung, die ausgewählte leichtflüchtige Substanzen enthält, dotiert. Die anschließende Stabilitätsuntersuchung mit den so hergestellten Proben zeigte, dass es notwendig ist, die Bodenproben mit einem organischen Lösungsmittel (z. B. Methanol) zu überschichten, um Verluste der leichtflüchtigen organischen Substanzen so gering wie möglich zu halten. Die Voruntersuchungen haben gezeigt, dass die Wiederfindungsraten von LHKW und BTEX in Boden ohne Überschichtung sehr schlecht sind. Das erarbeitete Analysenverfahren liegt als Normvorschlag dem Normausschuss ISO/TC 190 - Soil quality vor und wurde im Rahmen eines Ringversuches mit den hergestellten Referenzmaterialien erfolgreich validiert. Das validierte Verfahren mit den Verfahrenskenndaten wurde als ISO DIS 22155 im September 2003 aktualisiert. T3 - BAM Forschungsberichtreihe - 273 PY - 2005 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1789 SN - 978-3-86509-436-8 SN - 0938-5533 VL - 273 SP - 1 EP - 138 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-178 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Dorgerloh, Ute A1 - Win, Tin A1 - Becker, Roland A1 - Schultze, Karin A1 - Philipp, Rosemarie A1 - Redlich, Christel T1 - Entwicklung, Herstellung und Zertifizierung eines Referenzmaterials zur Bestimmung von Organochlorpestiziden in Boden T2 - Tag der Chemie, Wissenschaftspark Golm CY - Potsdam, Germany DA - 2000-11-08 PY - 2000 AN - OPUS4-5731 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Win, Tin A1 - Schultze, Karin A1 - Philipp, Rosemarie A1 - Redlich, Christel T1 - Entwicklung, Herstellung und Zertifizierung eines Referenzmaterials zur Bestimmung von Organochlorpestiziden in Boden T2 - Analytica Conference 2000 CY - Munich, Germany DA - 2000-04-11 PY - 2000 AN - OPUS4-5729 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schultze, Karin A1 - Becker, Roland A1 - Win, Tin A1 - Nehls, Irene T1 - Entwicklung, Herstellung und Zertifizierung eines Referenzmaterials zur Bestimmung von "Organochlorpestiziden in Boden" T2 - Tagung "Tag der Chemie" CY - Potsdam, Deutschland DA - 2000-11-08 PY - 2000 AN - OPUS4-1001 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Entwicklung, Herstellung und Einsatz von Referenzmaterialien für die organische Umweltanalytik T2 - Analytica Conference 2000 CY - München, Deutschland DA - 2000-04-11 PY - 2000 SP - 1(?) CY - München AN - OPUS4-939 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Entwicklung, Herstellung und Einsatz von Referenzmaterialien für die organische Umweltanalytik T2 - Analytica Conference 2000 CY - Munich, Germany DA - 2000-04-10 PY - 2000 AN - OPUS4-5760 LA - deu 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 UR - https://nbn-resolving.org/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 - TY - JOUR A1 - Köppen, Robert A1 - Becker, Roland A1 - Emmerling, Franziska A1 - Jung, Christian A1 - Nehls, Irene T1 - Enantioselective Preparative HPLC Separation of the HBCD-Stereoisomers from the Technical Product and Their Absolute Structure Elucidation Using X-Ray Crystallography N2 - 1,2,5,6,9,10-Hexabromocyclododecane (HBCD) is a widely used flame retardant, which tends to persist in the environment and accumulates in biota. The six stereoisomers (three racemates named α-, β-, and γ-HBCD) of the technical mixture were isolated with high-performance liquid chromatography (HPLC). Direct separations were performed on a chiral stationary phase containing permethylated -cyclodextrin (NUCLEODEX -PM column) and the pure enantiomers of α-, β-, and γ-HBCD were physically characterized for the first time. The absolute configurations of all six isomers were determined by anomalous dispersion using single crystal X-ray crystallography. Optical rotations αD in tetrahydrofuran were +4.2/-4.0 (α-HBCD), +26.1/-27.5 (β-HBCD), and +68.0/-66.3 (γ-HBCD). The sense of rotation could be correlated with the absolute configurations of α-, β-, and γ-HBCD enantiomers and their order of elution on a chiral permethylated β-cyclodextrin-bonded stationary phase. The diastereomers α-, β-, and γ-HBCD displayed distinctly different melting points as well as 1H-, 13C NMR, and IR spectra. KW - Brominated flame retardant KW - Chiral separation KW - Anomalous dispersion KW - Crystal structures KW - Optical rotation KW - Absolute configuration PY - 2007 DO - https://doi.org/10.1002/chir.20366 SN - 0899-0042 SN - 1520-636X VL - 19 IS - 3 SP - 214 EP - 222 PB - Wiley-Liss CY - New York, NY AN - OPUS4-14718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Köppen, Robert A1 - Becker, Roland A1 - Nehls, Irene T1 - Enantiomerenspezifischer Vergleich von HBCD-Gehalten maritimer Lebewesen zweier norwegischer Fjorde PY - 2010 SN - 0934-3504 SN - 1865-5084 VL - 22 IS - 4 SP - 441 PB - Springer CY - Heidelberg AN - OPUS4-22906 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Becker, Roland A1 - Esslinger, Susanne A1 - Nehls, Irene T1 - Enantiomer-specific analysis of hexabromocyclododecane in fish from Etnefjorden (Norway) N2 - High-performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS) was applied to sterospecifically quantify the content of α-, β-, and γ-hexabromocyclododecane (HBCD) in six fish species from the Norwegian Etnefjorden. A combination of a β-PM cyclodextrin and an achiral column enabled the paired chromatographic separation of the stereoisomers in the order (-)-α-, (+)-α-, (-)-β-, (+)-β-, (+)-γ- and, (-)-γ-HBCD. The limits of detection were in the range of 6–21 pg g-1 depending on the stereoisomer and the concentrations of α-, β-, and γ-HBCD in fillets ranged from <5.4 ng g-1 to 11.1 µg g-1 lipid weight. α-HBCD enantiomers were throughout dominating, and in most cases the accumulation of the respective first eluted enantiomers ((-)-α-, (-)-β- and (+)-γ-HBCD) was observed. Deviations from the racemic EF-value were considered to be significant if it was outside of the expanded uncertainty range for each of the racemic HBCD-ratios. The composition of HBCD isomers varied between the investigated fish species and the relative high values for the γ-HBCD concentrations for the bottom-dwellers flounder and thorny skate seems to echo the HBCD pattern of ocean sediments. KW - Flame retardant KW - Diastereomers KW - Chiral separation KW - Bioaccumulation KW - Enantiomeric fraction PY - 2010 DO - https://doi.org/10.1016/j.chemosphere.2010.06.019 SN - 0045-6535 SN - 0366-7111 VL - 80 IS - 10 SP - 1241 EP - 1245 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-22377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -