TY - CONF A1 - Nehls, Irene T1 - Lebensmittelanalytik - eine neue Herausforderung an die BAM T2 - Einladung zum Institutskolloquium, Institut für Landschaftsdynamik, Leibniz-Zentrum für Agrarlandschaftsforschung (ZALF) e. V. CY - Müncheberg, Germany DA - 2010-02-16 PY - 2010 AN - OPUS4-21058 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 - 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 - 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 - 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 DO - 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 - CONF A1 - Nehls, Irene T1 - Referenzmaterialien - Instrimente der Qualitätssicherung T2 - Kolloquium im Fachbereich Chemie der Humboldt-Universität Berlin auf Einladung von Herrn Prof. Linscheid CY - Berlin, Germany DA - 2004-02-24 PY - 2004 AN - OPUS4-5471 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 - 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 - 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 - 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 - 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 - Kuhlich, Paul A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Nehls, Irene A1 - Piechotta, Christian T1 - 1-(4-bromo-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethan-1-one: a precursor for phase-I metabolite of AHTN N2 - The title compound, C18H25BrO, crystallized as a racemate with four independent molecules in the asymmetric unit. In the crystal, three of these four molecules are linked via C-Br...Br-C halogen bonds [Br...Br = 3.662 (2) and 3.652 (2) Å], forming dimers. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-279935 DO - https://doi.org/10.1107/S1600536813006934 SN - 1600-5368 VL - 69 IS - 4 SP - o545, sup-1 EP - sup-17 PB - Munksgaard CY - Copenhagen AN - OPUS4-27993 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 - Kuhlich, Paul A1 - Emmerling, Franziska A1 - Piechotta, Christian A1 - Nehls, Irene T1 - Methyl 3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalene-2-carboxylate (AHTN-COOMe) N2 - Crystals of the title compound, C18H26O2, were grown from ethyl acetate. Due to the racemic precursor, the title compound is also obtained as a racemate. Disorder was observed during structure refinement, originating from two possible half-chair conformations of the non-aromatic ring. The disorder was refined by introducing split positions in the cyclo-hexane ring regarding the two possible R and S-enantiomers at the chiral CH group [ratio 0.744 (3):0.256 (3)]. The crystal structure features pairs of inversion-related molecules connected by pairs of non-classical C–H···O hydrogen bonds. KW - AHTN KW - Tonalide KW - Cyclic musk KW - AHTN-COOMe KW - Disinfection by-product KW - Esterification PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-232769 DO - https://doi.org/10.1107/S1600536811002601 SN - 1600-5368 VL - E67 IS - 2 SP - o485, sup-1 EP - sup-11 PB - Munksgaard CY - Copenhagen AN - OPUS4-23276 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 - Mönch, Bettina A1 - Gebert, Antje A1 - Emmerling, Franziska A1 - Becker, Roland A1 - Nehls, Irene T1 - Koenigs-Knorr reaction of fusel alcohols with methyl (1-bromo-2,3,4-tri-O-acetyl-alpha-D-glucopyranosid)uronate leading to the protected alkyl glucuronides-crystal structures and high resolution 1H and 13C NMR data N2 - Crystal structures and high resolution 1H and 13C NMR spectral data for methyl (alkyl 2,3,4-tri-O-acetyl-β-D-glucopyranosid)uronates (alkyl = methyl, ethyl, n-propyl, i-propyl, n-butyl, sec-butyl, i-butyl, n-pentyl, 2-methyl-1-butyl and 3-methyl-1-butyl) are presented. KW - D-Glucuronic acid derivates KW - X-ray analysis KW - High resolution NMR KW - Anomeric configuration KW - Synthesis PY - 2012 DO - https://doi.org/10.1016/j.carres.2012.01.002 SN - 0008-6215 SN - 1873-426X VL - 352 SP - 186 EP - 190 PB - Elsevier CY - Amsterdam AN - OPUS4-25759 LA - eng 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 - CONF A1 - Köppen, Robert A1 - Becker, Roland A1 - Emmerling, Franziska A1 - Jung, Christian A1 - Nehls, Irene T1 - HBCD enantiomers: absolute configurations and thermal rearrangement T2 - Organohalogen Compounds PY - 2006 UR - http://www.dioxin20xx.org/pdfs/2006/06-466.pdf VL - 68 SP - 1991 EP - 1994 PB - Norwegian Institute of Public Health AN - OPUS4-14540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siegel, David A1 - Troyanov, S. A1 - Noack, J. A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Alternariol N2 - In the title compound (systematic name: 3,7,9-trihydroxy-1-methyl-6H-benzo[c]chromen-6-one), C14H10O5, the methyl group is shifted out of the molecular plane due to a steric collision, thus causing a slight twist of the benzene rings. The molecular structure is stabilized by an intramolecular O-H...O hydrogen bond, generating an S(6) ring. In the crystal, molecules are connected by intermolecular O-H...O hydrogen bonds into a three-dimensional network. KW - Alternariol KW - Kristallstruktur PY - 2010 DO - https://doi.org/10.1107/S1600536810017502 SN - 1600-5368 VL - 66 IS - 6 SP - o1366 PB - Munksgaard CY - Copenhagen AN - OPUS4-21400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -