TY - JOUR A1 - Becker, Roland A1 - Buge, Hans-Gerhard A1 - Bremser, Wolfram A1 - Nehls, Irene T1 - Mineral oil content in sediments and soils: comparability, traceability and a certified reference material for quality assurance N2 - The performance of twelve laboratories with previously established proficiency in the determination of the mineral oil content in a fresh water sediment is described. The summation parameter total petrol hydrocarbon (TPH) is defined according to ISO 16703:2004 with regard to the sample preparation to be applied, the flame ionisation detection (FID) and the boiling range of C10–C40 to be integrated. Comprehensive tests of homogeneity and stability have been carried out on the candidate material using appropriate models. The outcome of the study served as the basis for the certification of the candidate reference material as ERM-CC015a. The certified mass fraction is 1,820±130mgkg-1 and traceability was established by using an appropriate calibration standard certified for the mass fraction of C10–C40. The interlaboratory scatter of measurement results in this exercise can largely be explained by the variability of the individual calibrations based on this common calibration standard. KW - Total petroleum hydrocarbons KW - Extraction KW - Gas chromatography KW - Calibration KW - Interlaboratory study PY - 2006 DO - https://doi.org/10.1007/s00216-006-0423-4 SN - 1618-2642 SN - 1618-2650 VL - 385 IS - 3 SP - 645 EP - 651 PB - Springer CY - Berlin AN - OPUS4-12399 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 - RPRT A1 - Schwarzer, Martin A1 - Becker, Roland A1 - Kuhnhardt, Claus A1 - Nehls, Irene T1 - Methodenvergleich zur Bestimmung von extrahierbaren organischem Halogen (EOX) in Bodenproben N2 - Ziel der vorliegenden Untersuchungen, die im Rahmen einer Diplomarbeit der Fachhochschule Lausitz/Senftenberg an der BAM durchgeführt wurden, war ein Vergleich unterschiedlicher Extraktionsverfahren für die Bestimmung von extrahierbarem organischem Halogen (EOX) in Bodenproben. EOX ist ein für die rasche Bewertung der Organochlor- Belastung kontaminationsverdächtiger Flächen wertvoller Summenparameter, der sämtliche mit organischen Lösungsmittel extrahierbare Organohalogenverbindungen erfasst. Gegenwärtig existiert jedoch kein für die Bodenanalytik genormtes Verfahren für die Durchführung von EOX-Bestimmungen. Daher wird in der Praxis auf das für Schlämme und Sedimente entwickelte Verfahren nach DIN 38414 S17 (1990) zurückgegriffen, so auch in der Bundesbodenschutz- und Altlasten-Verordung (BBodSchV). Literaturangaben und Erfahrungen mit der Wiederfindungsrate polarer Extraktionsmittel und moderner Extraktionsverfahren bei Organochlorpestiziden, die eine bedeutende Quelle für EOX in Schlämmen und Böden darstellen, lassen vermuten, dass das genannte Normverfahren systematisch zu Unterbefunden neigen könnte. Für die Untersuchungen wurden an der BAM entwickelte Boden-Referenzmaterialien mit "natürlicher", über jahrzehntelangen Eintrag entstandener DDT- und Lindan-Belastung verwendet. Neben den klassischen Extraktionsverfahren nach Soxhlet kamen die ultraschallunterstützte Extraktion, die Mikrowellen- und die beschleunigte Lösungsmittelextraktion (ASE) jeweils mit Lösungsmitteln unterschiedlicher Polarität zum Einsatz. Extraktionsausbeuten und Wiederholpräzision der einzelnen Varianten wurden verglichen und vor dem Hintergrund der Ergebnisse unabhängiger Verfahren wie der gaschromatographischen Bestimmung der einzelnen Organochlorverbindungen bewertet. Die Polarität des Extraktionsmittels weist auch bei trockenen Böden den größten Einfluss auf die Extraktionsausbeuten der in den untersuchten Proben enthaltenen Organochlorverbindungen auf. Die Mischung Hexan/Aceton (1:1), die sich für die Extraktion verschiedener organischer Parameter bewährt hat, ist hinsichtlich der EOX-Analytik der existierenden Norm überlegen. T3 - BAM Forschungsberichtreihe - 263 PY - 2003 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1884 SN - 978-3-86509-083-4 SN - 0938-5533 VL - 263 SP - 1 EP - 64 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Jancke, Harald A1 - Nehls, Irene T1 - Messung und Quantifizierung von Mineralölkohlenwasserstoffen - Ein Vergleich von FT/IR, GC-FID und 1H-NMR KW - H-1-Kernresonanz-Spektroskopie KW - H-1-NMR KW - Fourier-Transform-Infrarot-Spektroskopie KW - FT/IR KW - GC-FID KW - Kapillargaschromatographie-Flammenionisationsdetektion KW - MKW KW - Mineralölkohlenwasserstoffe KW - Umweltanalytik PY - 1999 SN - 0934-3504 SN - 1865-5084 VL - 11 IS - 1 SP - 9 EP - 14 PB - Springer CY - Heidelberg AN - OPUS4-7041 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 - 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 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 - 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 lumiergometrine could 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 - Neuhof, Torsten A1 - Köppen, Robert A1 - Koch, Matthias A1 - Nehls, Irene T1 - Letter: High-performance liquid chromatography/electrospray mass spectrometry analysis of the mycotoxin aurofusarin N2 - High-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) can be used for simultaneous quantification of various mycotoxins in contaminated food samples. Therefore, multi-mycotoxin methods have been developed in the last couple of years. To enlarge these methods for further analytes, we have developed a LC-MS/MS method for the quantification of the mycotoxin aurofusarin. Additionally, further LC-MSn experiments were performed to demonstrate the fragmentation pattern of aurofusarin. Applicable multiple reaction monitoring (MRM) transitions of aurofusarin were found and optimized by parameter variation of the tandem mass spectrometer. The applicability of the developed method was tested by analysis of naturally contaminated wheat. KW - LC-MS/MS KW - Multi-mycotoxin method KW - Aurofusarin PY - 2008 DO - https://doi.org/10.1255/ejms.935 SN - 1469-0667 SN - 1356-1049 SN - 1365-0718 VL - 14 IS - 5 SP - 329 EP - 333 PB - IM Publications CY - Chichester AN - OPUS4-18199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Neuhof, Torsten A1 - Nehls, Irene ED - Jörg Peter Matthes, ED - Markus Frasch, ED - Marx, Wolfram ED - Johannes Oeler, T1 - Lebensmittelanalytik - Neue Referenzmaterialien KW - Referenzmaterialien KW - Acrylamid KW - Ochratoxin A KW - Methylquecksilber PY - 2007 VL - 3 IS - 5 SP - 16 EP - 17 PB - Succidia Verl. & Kommunikation CY - Darmstadt AN - OPUS4-16691 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Koch, Matthias A1 - Köppen, Robert A1 - Siegel, David A1 - Merkel, Stefan A1 - Piechotta, Christian A1 - Becker, Roland A1 - Win, Tin T1 - Lebensmittelanalytik - eine neue Herausforderung für die BAM T2 - Lebensmittelchemisches Kolloquium der Universität Hohenheim CY - Stuttgart, Germany DA - 2009-11-19 PY - 2009 AN - OPUS4-20584 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Koch, Matthias A1 - Köppen, Robert A1 - Siegel, David A1 - Merkel, Stefan A1 - Piechotta, Christian A1 - Becker, Roland A1 - Win, Tin 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 - 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 - 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 - Mönch, Bettina A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Becker, Roland A1 - Nehls, Irene T1 - Isopropyl 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranoside N2 - The title compound, C17H26O10, was formed by a Koenigs-Knorr reaction of 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl bromide and propan-2-ol. The central ring adopts a chair conformation. The crystal does not contain any significant intermolecular interactions. PY - 2013 DO - https://doi.org/10.1107/S1600536812051483 SN - 1600-5368 VL - 69 IS - Part 2 SP - o157, sup-1 - sup-7 PB - Munksgaard CY - Copenhagen AN - OPUS4-27572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Retter, Utz A1 - Koch, Matthias A1 - Nehls, Irene T1 - Investigation of the optimization of the recovery of mineral oil from water N2 - A method has been derived to completely recover mineral oil dispersed in water. The method involves three steps: the emulsification of the mineral oil by adding amphiphiles, the breaking of the emulsion by adding salts and the extraction of the mineral oil by a non-polar aprotic solvent. Various amphiphiles and types and concentrations of salts were tested. By using amphiphiles with HLB numbers in the range 4.7 to 40 a complete recovery of the mineral oil could be obtained for a combination of salts Na2SO4 + NaH2PO4 with total ionic strength of 6 mol/L. PY - 1999 SN - 0937-0633 VL - 364 SP - 777 EP - 779 PB - Springer CY - Berlin AN - OPUS4-7524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Becker, Roland A1 - Jung, Christian A1 - Piechotta, Christian A1 - Nehls, Irene T1 - Investigation of extraction procedures and HPLC-DAD/MS for the determination of the brominated flame retardant tetrabromobisphenol A bis(2,3-dibromopropylether) in environmental samples N2 - A method for the determination of the novel brominated flame retardant tetrabromobisphenol A bis(2,3-dibromopropylether), 1,1'-(isopropylidene)bis[3,5-dibromo-4-(2,3-dibromo-propoxy)-benzene] (TBBPA-dbpe), was developed. Technical TBBPA-dbpe was purified and the results of a thorough physical characterisation are reported. The application of APCI-MS is discussed and the fragmentation patterns are described. Quantification of TBBPA-dbpe was done by HPLC-DAD using external calibration. The validation of the method was accomplished using sediment and sewage sludge samples spiked with defined amounts of authentic TBBPA-dbpe. The average recovery rates of TBBPA-dbpe from spiked samples ranged from 35 to 91% (sediment) and from 57 to 98% (sewage sludge) depending on the respective extraction method. Pressurised fluid extraction (PFE) and fluidised bed extraction were superior to classical Soxhlet and sonication procedures and yielded recovery rates between 90 and 98% with relative standard deviations of 2%. The limits of detection (DTC), identification (ID) and determination (DTM) using HPLC-DAD were 10, 21 and 30 ng g-1 in sediment and 22, 44 and 72 ng g-1 in sewage sludge, respectively. KW - Extraction KW - TBBPA-dbpe KW - Sewage sludge KW - Sediment KW - LC-MS KW - Mass spectrometry KW - APCI KW - HPLC-DAD PY - 2006 DO - https://doi.org/10.1007/s00216-006-0339-z SN - 1618-2642 SN - 1618-2650 VL - 384 IS - 7-8 SP - 1485 EP - 1492 PB - Springer CY - Berlin AN - OPUS4-12255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Nehls, Irene A1 - Dorgerloh, Ute T1 - Interlaboratory comparisons - demonstrating degree of equivalence N2 - The role of matrix reference materials in the process of demonstrating the degree of equivalence of measurement results obtained from intercomparisons is outlined, reviewing exemplary selected experience gained at BAM regarding the determination of organic contaminants in environmental matrices. The specific characteristics of reference materials employed in the process of demonstrating equivalence between laboratories in the course of proficiency testing as well as the development, comparison and validation of methods are elaborated. The demand is for series of appropriately characterised samples which are fit for the purpose and it is seen from representative examples that the utilisation of such tailor-made RM designed to tackle the specific need of an analytical problem dominates over certified matrix reference materials in this context. Concluding, the role of certified matrix reference materials in quality assurance is briefly looked at both from the user’s and providers’ points of view. KW - Certification KW - Equivalence KW - Method development KW - Proficiency testing KW - Reference materials PY - 2003 DO - https://doi.org/10.1007/s00769-003-0580-5 SN - 0949-1775 SN - 1432-0517 VL - 8 SP - 150 EP - 155 PB - Springer CY - Berlin AN - OPUS4-2848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Zwaka, H. A1 - Menzel, R. A1 - Johnen, D. A1 - Fischer-Tenhagen, C. A1 - Rolff, J. A1 - Nehls, Irene T1 - In vitro cultured lung cancer cells are not suitable for animal-based breath biomarker detection N2 - In vitro cultured lung cancer cell lines were investigated regarding the possible identification of volatile organic compounds as potential biomarkers. Gas samples from the headspace of pure culture medium and from the cultures of human lung adenocarcinoma cell lines A549 and Lu7466 were exposed to polypropylene fleece in order to absorb odour components. Sniffer dogs were trained with loaded fleeces of both cell lines, and honey bees were trained with fleeces exposed to A549. Afterwards, their ability to distinguish between cell-free culture medium odour and lung cancer cell odour was tested. Neither bees nor dogs were able to discriminate between odours from the cancer cell cultures and the pure culture medium. Solid phase micro extraction followed by gas chromatography with mass selective detection produced profiles of volatiles from the headspace offered to the animals. The profiles from the cell lines were largely similar; distinct differences were based on the decrease of volatile culture medium components due to the cells' metabolic activity. In summary, cultured lung cancer cell lines do not produce any biomarkers recognizable by animals or gas chromatographic analysis. KW - A549 KW - Honey bees KW - Odour discrimination task KW - Sniffer dogs KW - Solid phase microextraction KW - Volatile organic compounds KW - Volatilome PY - 2015 DO - https://doi.org/10.1088/1752-7155/9/2/027103 SN - 1752-7155 SN - 1752-7163 VL - 9 IS - 2 SP - 027103-1 EP - 027103-10 PB - IOP CY - Bristol AN - OPUS4-34161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Helmis, M. A1 - Mumme, J. A1 - Diakité, M. A1 - Nehls, Irene T1 - Hydrothermally carbonized plant materials: Patterns of volatile organic compounds detected by gas chromatography N2 - The nature and concentrations of volatile organic compounds (VOCs) in chars generated by hydrothermal carbonization (HTC) is of concern considering their application as soil amendment. Therefore, the presence of VOCs in solid HTC products obtained from wheat straw, biogas digestate and four woody materials was investigated using headspace gas chromatography. A variety of potentially harmful benzenic, phenolic and furanic volatiles along with various aldehydes and ketones were identified in feedstock- and temperature-specific patterns. The total amount of VOCs observed after equilibration between headspace and char samples produced at 270 °C ranged between 2000 and 16,000 µg/g (0.2–1.6 wt.%). Depending on feedstock 50–9000 µg/g of benzenes and 300–1800 µg/g of phenols were observed. Substances potentially harmful to soil ecology such as benzofurans (200–800 µg/g) and p-cymene (up to 6000 µg/g in pine wood char) exhibited concentrations that suggest restrained application of fresh hydrochar as soil amendment or for water purification. KW - Hydrochar KW - Mass spectrometry KW - Flame ionization detection KW - Phenols KW - Benzenes PY - 2013 DO - https://doi.org/10.1016/j.biortech.2012.12.102 SN - 0960-8524 SN - 1873-2976 VL - 130 SP - 621 EP - 628 PB - Elsevier Applied Science CY - Barking, Essex AN - OPUS4-27616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Paulke, E. A1 - Mumme, J. A1 - Nehls, Irene T1 - Hydrothermal carbonization of biomass: Major organic components of the aqueous phase N2 - Process waters obtained from hydrothermal carbonization (HTC) of wheat straw, a biogas digestate derived thereof, and four woody biomass feedstocks were quantified regarding the total organic carbon (TOC) and selected organic compounds. HTC runs revealed that TOC loads were largely unaffected by process severity or type of feedstock whereas the C2–C6 fatty acids, determined by GC, displayed clear effects of temperature and feedstock. HPLC demonstrated simultaneously the initial increase and subsequent consumption of cellulose-derived furfural and 5-hydroxymethylfurfural as well as the increase of the lignin-derived 2-methoxyphenol. 2-Methylbenzofuran, an example for a substance potentially harmful to aquatic biota, was observed in high concentration in the HTC liquor from wheat straw-based feedstocks. KW - Furfurals KW - Gas chromatography KW - Liquid chromatography KW - Phenols KW - Process water KW - Total organic carbon PY - 2014 DO - https://doi.org/10.1002/ceat.201300401 SN - 0930-7516 SN - 1521-4125 VL - 37 IS - 3 SP - 511 EP - 518 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-30333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Lutz, A. A1 - Bremser, Wolfram A1 - Hilbert, S. A1 - Nehls, Irene T1 - How to improve reliability in groundwater analysis: over a decade of experience with external quality control in field campaigns on volatile halogenated compounds N2 - The reliability in measurement results obtained during environmental monitoring is crucial for the assessment and further planning of remediation efforts on the respective contaminated sites by the responsible authorities. A case study concerned with groundwater contaminated with perchloroethylene, trichloroethylene and 1,1,2-trichlorotrifluoroethane including their degradation products which involves private contract laboratories and an independent provider of quality assurance (QA) is presented. The experience gained with biannual monitoring campaigns over 14 years indicates that the selection of contractors on basis of accreditation status and successful performance in interlaboratory comparisons are not sufficient. Rather the auditing of the contractors by the QA provider prior to each campaign and the crosschecking of selected monitoring samples by the QA provider led to a lasting improvement of reliability in the contractors' measurement results. A mean deviation of 20% from the reference value determined by the QA provider for the crosschecked samples was reached. KW - Groundwater monitoring KW - External quality management KW - QM KW - VOC PY - 2012 DO - https://doi.org/10.1039/c1em10460h SN - 1464-0325 SN - 1464-0333 VL - 14 IS - 1 SP - 217 EP - 223 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-25288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Maul, Ronald A1 - Nehls, Irene T1 - Hexabromocyclododecane enantiomers: microsomal degradation and patterns of hydroxylated metabolites N2 - The degradation of the enantiomers of α-, β-, and γ-hexabromocyclododecane (HBCD) by phase I metabolism was investigated using induced rat liver microsomes. HBCD isomers were quantified using HPLC-MS/MS (ESI-) after separation on a combination of a reversed phase and a chiral analytical column. The degradation of all six isomers followed first-order kinetics and the estimated half-lives ranged from 6.3 min for both β-HBCD enantiomers to 32.3 min in case of (+)-γ-HBCD. (+)-α- and (–)-γ-HBCD displayed significantly shorter half-lives than their corresponding antipodes. It could be shown that this degradation led to a significant enrichment of the first eluting enantiomers (–)-α- and (+)-γ-HBCD. Individual patterns of mono- and dihydroxylated derivatives obtained from each α- and γ-HBCD enantiomer were seen to be distinctly characteristic. The patterns of monohydroxylated HBCD derivatives detected in liver and muscle tissues of pollack, mackerel and in herring gull eggs were largely similar to those observed in the in vitro experiments with rat liver microsomes. This enabled individual hydroxy-HBCDs to be assigned to their respective parent HBCD enantiomers. KW - Brominated flame retardant KW - Cytochromes KW - Phase I metabolism KW - Hydroxylation KW - HPLC-MS/MS PY - 2011 DO - https://doi.org/10.1021/es1039584 SN - 0013-936X SN - 1520-5851 VL - 45 IS - 9 SP - 3938 EP - 3944 PB - ACS Publ. CY - Washington, DC AN - OPUS4-23837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Nehls, Irene T1 - Hexabromcyclododecan in heimischen Süßwasserfischen N2 - Hexabromcyclododecan senkt als Flammschutzmittel die Entflammbarkeit von Polymeren und verhindert damit Brände. Als persistente Verbindung reichert es sich in der belebten und in der unbelebten Umwelt an und steht daher im Fokus öffentlichen Interesses. PY - 2009 DO - https://doi.org/10.1002/nadc.200967612 SN - 1439-9598 SN - 1521-3854 VL - 57 IS - 9 SP - 901 EP - 904 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-19911 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Maul, Ronald A1 - Nehls, Irene T1 - Hexabromcyclododecan - Untersuchungen zum Phase I Metabolismus PY - 2010 SN - 0934-3504 SN - 1865-5084 VL - 22 IS - 4 SP - 364 PB - Springer CY - Heidelberg AN - OPUS4-22907 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Herstellung und Zertifizierung von Referenzmaterialien für die organische Analytik T2 - Schering AG CY - Berlin, Germany DA - 2001-03-07 PY - 2001 AN - OPUS4-5820 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Herstellung und Zertifizierung von BAM-Referenzmaterialien und ihr Einsatz als Instrument der Qualitätssicherung in chemischen Laboratorien T2 - Einladung zum GDCh-Kolloquium an der Friedrich-Schiller-Universität CY - Jena, Germany DA - 2003-06-11 PY - 2003 AN - OPUS4-5863 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Köppen, Robert A1 - Becker, Roland A1 - Weber, M. A1 - Durmaz, V. A1 - Nehls, Irene T1 - HBCD stereoisomers: Thermal interconversion and enantiospecific trace analysis in biota T2 - DIOXIN 2008, 28th International Symposium on Halogenated Persistent Organic Pollutants (POPs) CY - Birmingham, UK DA - 2008-08-17 KW - HBCD KW - Stereoisomerie KW - Persistent Organic Pollutant KW - HPLC-MS PY - 2008 UR - http://www.dioxin20xx.org/pdfs/2008/08-819.pdf IS - Paper #154 SP - 1 EP - 4 AN - OPUS4-17842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Müller-Belecke, A. A1 - Bremser, Wolfram A1 - Jung, Christian A1 - Nehls, Irene T1 - HBCD stereoisomer pattern in mirror carps following dietary exposure to pure Gamma-HBCD enantiomers KW - Enantiomer-specific determination KW - HPLC-MS/MS KW - Brominated flame retardant KW - Fish feeding experiment KW - Enantiomer fraction KW - Bioisomerization PY - 2010 DO - https://doi.org/10.1021/jf101469q SN - 0021-8561 SN - 1520-5118 VL - 58 IS - 17 SP - 9705 EP - 9710 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-23173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Nehls, Irene T1 - HBCD isomers: degradation rates and hydroxylated products from microsome incubation experiments T2 - Dioxin 2010 - 30th International symposium on halogenated persistent organic pollutants CY - San Antonio, TX, USA DA - 2010-09-12 PY - 2010 UR - http://www.dioxin20xx.org/pdfs/2010/10-1113.pdf N1 - Serientitel: Organohalogen Compounds – Series title: Organohalogen Compounds VL - 72 SP - 259 EP - 262 AN - OPUS4-23168 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 - RPRT A1 - Koch, Matthias A1 - Win, Tin A1 - Hoffmann, Andrea A1 - Nehls, Irene T1 - Gezielte Untersuchung und Optimierung der Verfahrensschritte für die gas-chromatographische Bestimmung von Mineralölkohlenwasserstoffen in Feststoffen aus dem Altlastenbereich nach der Methode des FGAA N2 - Ziel des Forschungsprojektes war es, systematische Untersuchungen der Verfahrensschritte für die gas-chromatographische Bestimmung von Mineralölkohlenwasserstoffen (MKW) in Feststoffen aus dem Altlastenbereich entsprechend der Methode des Fachgremiums Altlastenanalytik (FGAA) sowie des Verfahrens ISO/DIS 16703 durchzuführen, Wege zur Optimierung einzelner Verfahrensschritte aufzuzeigen und beide Verfahren miteinander zu vergleichen. Es wurden Untersuchungen zu den Verfahrensschritten Extraktion, Extraktreinigung, Messung und Integration durchgeführt. Im Ergebnis der Untersuchungen wurde festgestellt, dass die Extraktion von Feststoffproben (20 g) mit einem Extraktionsvolumen von mind. 40 mL Aceton und 20 mL n-Heptan erfolgen muss, um eine zufriedenstellende Extraktionsausbeute zu gewährleisten. Im Rahmen dieses Projektes wurde ein Rechenprogramm für die Bestimmung der Rest- Aceton-Konzentration in Heptan-Extrakten erstellt. Mit diesem Programm können auch die Wasservolumina ermittelt werden, die für eine gewünschte Rest-Aceton-Konzentration notwendig sind. Anhand von Bodenextrakten, PAK-, Stearylstearat- und Triglycerid-Standardlösungen wurde nachgewiesen, dass die Säulen-Technik eine wesentlich effektivere Extraktreinigung bewirkt als das sogenannte Batch-(Schüttel-) Verfahren. In einem Modellversuch an drei verschiedenen Bodenextrakten wurde gezeigt, dass die zwischen FGAA- und ISO-Verfahren unterschiedliche Art der Peak-Integration eines GC-FID Chromatogramms zwischen n-Dekan (C10) und n-Tetracontan (C40) keinen Einfluss auf das Endergebnis hat. Eine Basislinienkorrektur des Proben-Chromatogramms ist daher nicht erforderlich. Das FGAA-Verfahren enthält in seiner Vorschrift für die Berechnung des MKW-Gehalts im Probenmaterial einen systematischen Fehler von etwa 8 %. Dieser Fehler entsteht durch den Unterschied zwischen dem theoretischen Extraktvolumen von 150 mL und dem realen Extraktvolumen von etwa 139 mL. Dieser systematische Fehler sollte in einer nachfolgenden Fassung des FGAA-Verfahrens vermieden werden. T3 - BAM Forschungsberichtreihe - 262 PY - 2003 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1895 SN - 978-3-86509-036-2 SN - 0938-5533 VL - 262 SP - 1 EP - 36 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-189 LA - deu 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 - 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 - TY - CONF A1 - Nehls, Irene T1 - Einsatz der hochauflösenden Flüssigkeits-NMR-Spektroskopie in der Celluloseforschung T2 - ZELLCHEMING CY - Baden-Baden, Germany DA - 1994-05-24 PY - 1994 AN - OPUS4-5611 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Lehnik-Habrink, Petra A1 - Hein, Sebastian A1 - Philipp, Rosemarie A1 - Nehls, Irene A1 - Win, Tin T1 - Einarbeitung und Validierung von Verfahren zur Bestimmung von polychlorierten Biphenylen und polychlorierten Terphenylen in organischen Materialien N2 - ISBN: Im Zuge der Harmonisierung der Rechtsvorschriften der Mitgliedsstaaten der Europäischen Gemeinschaft wurde im September 1996 die Richtlinie 96/59/EG des Rates über die Beseitigung polychlorierter Biphenyle und polychlorierter Terphenyle (PCB/PCT) verabschiedet. Ziel dieser Richtlinie ist die Angleichung der Rechtsvorschriften der Mitgliedstaaten über die kontrollierte Beseitigung der PCB, die Dekontaminierung oder Beseitigung PCB-haltiger Geräte und die Beseitigung von PCB-Abfall. In der Bundesrepublik Deutschland wurde mit der Verabschiedung der PCB/PCT- Abfallverordnung vom 26. Juni 2000 die EU-Richtlinie umgesetzt. Entsprechend der PCB/PCT-Abfallverordnung wird für PCB-haltigen Abfall ein Grenzwert von 50 mg/kg festgelegt. Beim Haupteinsatzgebiet der PCB - als Isolierflüssigkeiten in Transformatoren - ist die Bestimmung des PCB-Gehaltes durch DIN-Normen geregelt. Polychlorierte Biphenyle wurden auch als Weichmacher in Dichtungsmassen und Kunststoffen, z.B. in Kabelummantelungen, und als Flammschutzmittelanstrich für Holz eingesetzt. Für feste Abfallmatrices gibt es keine verbindliche Prüfvorschrift. Ziel des Projektes war die Erarbeitung und Validierung eines Prüfverfahrens zur Bestimmung von PCB und PCT in organischen Abfallmatrices wie Kabelshredder und Altholz. T3 - BAM Forschungsberichtreihe - 274 PY - 2006 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1773 SN - 978-3-86509-481-3 SN - 0938-5533 VL - 274 SP - 1 EP - 55 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-177 LA - deu 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 DO - 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 - Neuhof, Torsten A1 - Koch, Matthias A1 - Rasenko, Tatjana A1 - Nehls, Irene T1 - Distribution of Trichothecenes, Zearalenone, and Ergosterol in a Fractionated Wheat Harvest Lot N2 - To investigate possible co-occurrences of type B trichothecenes and zearalenone within a Fusarium culmorum-infected wheat harvest lot, kernels were fractionated into six groups by visual criteria. The Fusarium-damaged kernels were subdivided into white, shrunken, and red kernel groups, and the remaining kernels were sorted into healthy, black spotted, and nonspecific groups. The distribution patterns of nivalenol, deoxynivalenol, zearalenone, and ergosterol were determined for possible correlations. Significant correlations between the distribution patterns were found for the mycotoxins and ergosterol for the grouped kernels (r = 0.997-0.999, p < 0.0001). Additionally, remarkably outstanding levels of nivalenol (24-fold more than the mean at 1.16 mg/kg), deoxynivalenol (27-fold more than the mean at 0.16 mg/kg), zearalenone (25-fold more than the mean at 77 µg/kg), and ergosterol (17-fold more than the mean at 13.4 mg/kg) were found in the red kernel group. Further, detailed mycotoxin and ergosterol analyses were carried out on various segments (kernel surface, conidia, bran, and flour) of the red kernels. However, the mycotoxin and ergosterol distribution profiles revealed nonsignificant correlations for these kernel segments, with the exception of deoxynivalenol and nivalenol, which were moderately correlated (r = 0.948, p = 0.035). KW - Mycotoxins KW - Fusarium-damaged kernels KW - Ergosterol KW - Wheat KW - Correlation KW - HPLC-FLD/DAD PY - 2008 DO - https://doi.org/10.1021/jf800971q SN - 0021-8561 SN - 1520-5118 VL - 56 IS - 16 SP - 7566 EP - 7571 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-18196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Die sinnvolle Verwendung von zertifizierten Referenzmaterialien im Labor T2 - EURACHEM-CH CY - Zurich, Switzerland DA - 1999-07-01 PY - 1999 AN - OPUS4-5716 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Koch, Matthias A1 - Piechotta, Christian T1 - Die HPLC im Spannungsfeld zwischen Normung und Forschung T2 - Festkolloquium zu Ehren Dr. H. Knauer (80. Geburtstag) CY - Berlin, Germany DA - 2011-09-13 PY - 2011 AN - OPUS4-25164 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Win, Tin A1 - Lehnik-Habrink, Petra T1 - Die Bedeutung von Ringversuchen als Instrument der Qualitätssicherung und der Zertifizierung von Referenzmaterialien T2 - Analytica Conference '96 CY - Munich, Germany DA - 1996-04-23 PY - 1996 AN - OPUS4-5617 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Die Bedeutung von Matrix-Referenzmaterialien für die organische Umweltanalytik T2 - GDCh-Tagung Umwelt und Chemie und Jahrestagung des Arbeitskreises, Chromatografie CY - Karlsruhe, Germany DA - 1998-09-28 PY - 1998 AN - OPUS4-5698 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schultze, Karin A1 - Philipp, Rosemarie A1 - Redlich, Christel A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Win, Tin A1 - Nehls, Irene T1 - Development, preparation and certification of a reference material for the determination of chlorinated pesticides in soil T2 - Symposium "Reference Materials for Technologies in the New Millenium" CY - Berlin, BAM, Germany DA - 2000-05-22 PY - 2000 SP - 1(?) EP - 4(?) AN - OPUS4-1313 LA - eng 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 - Development, Preparation and Certification of a Reference Material for the Determination of Chlorinated Pesticides in Soil T2 - EUROLAB-Symposium CY - Berlin, Germany DA - 2000-05-22 PY - 2000 AN - OPUS4-5734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Bremser, Wolfram A1 - Köppen, Robert A1 - Siegel, David A1 - Töpfer, Antje A1 - Nehls, Irene T1 - Development of two certified reference materials for acrylamide determination in foods N2 - Certified reference materials (CRMs) are a versatile tool for quality assurance in the chemical laboratory. In the case of acrylamide analysis, the availability of appropriate materials was rather limited. This lack of acrylamide matrix CRMs has now been overcome by the development of two European reference materials (ERM) for the determination of acrylamide in food (crispbread, ERM-BD272, and rusk, ERM-BD274). This article describes the preparation of the materials, provides the results of the homogeneity and stability studies, and presents and discusses the outcome of the certification studies. Expert laboratories from different European countries took part in the certification studies using various analytical methods. The acrylamide mass fractions were certified to 980 µg kg-1 for crispbread and 74 µg kg-1 for rusk. KW - Certified reference materials KW - ERM KW - Acrylamide KW - Crispbread KW - Rusk KW - Quality assurance KW - Homogeneity KW - Stability PY - 2009 DO - https://doi.org/10.1021/jf901329t SN - 0021-8561 SN - 1520-5118 VL - 57 IS - 18 SP - 8202 EP - 8207 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-19888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Nehls, Irene T1 - Determination of volatile organic sulfur compounds in contaminated groundwater N2 - A practical method for the quantification of total purgeable organic sulfur (POS) in highly contaminated groundwater is described. Volatile organic sulfur compounds (VOSC) are purged from the water samples by a stream of oxygen and combusted. The emerging sulfur dioxide is absorbed in H2O2 and converted to sulfate which is quantified by ion chromatography and reported as mass sulfur equivalent. The overall limit of quantification is 0.03 mg l–1. The content of POS is balanced with the total VOSC determined by GC-AED after liquid–liquid extraction. Separate determination of the non-volatile organic sulfur compounds by direct combustion of the water sample and adsorption to charcoal yielded a mass balance of the total sulfur content. Semi-quantitative GC-MS after purge & trap accumulation revealed that the VOSC mixture is composed of C1–C4 alkyl sulfides. The implementation of the developed methodology for the quantification of VOSC as potential catalyst poison in a cleaning plant for groundwater contaminated with volatile haloorganics (VOX) is presented. KW - Contamination KW - Remediation KW - Summation parameter KW - Combustion KW - Ion chromatography KW - GC-AED KW - GC-MS PY - 2008 UR - http://www.springerlink.com/content/8612g42hwj7130g8/fulltext.pdf DO - https://doi.org/10.1007/s10311-007-0117-y SN - 1610-3653 SN - 1610-3661 VL - 6 IS - 2 SP - 101 EP - 106 PB - Springer CY - Berlin AN - OPUS4-16360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Köppen, Robert A1 - Siegel, David A1 - Witt, Angelika A1 - Nehls, Irene T1 - Determination of total sulfite in wine by ion chromatography after in-sample oxidation N2 - Sulfur dioxide (SO2) or sulfites are the most common preservatives used in winemaking. The level of total SO2 is subject to regulation. Currently, the regulatory determination of total SO2 (including sulfites) is done by the optimized Monier–Williams (OMW) method, which includes time-consuming distillation and titration steps. This paper describes the development and application of an alternative, rapid, straightforward, and reliable method for the determination of total sulfite in wine. In this method, a simple oxidation step using alkaline hydrogen peroxide (H2O2) solution is followed by ion chromatographic (IC) analysis of sulfate coupled with conductometric detection. Thirteen wines were analyzed in order to compare the in-sample oxidation method with the OMW-procedure. A t-test revealed satisfying compliance regarding sample preparation, i.e., alkaline H2O2 treatment and acidic distillation (OMW method). Comparable results were also obtained between IC analysis and acid/base titration. Our results indicate that the novel method (limit of quantification: 4 mg SO2 L-1) is well suited for the cost-efficient monitoring of regulatory limits. KW - Sulfur dioxide KW - Wine analysis KW - Hydrogen peroxide oxidation KW - IC KW - Optimized Monier-Williams method PY - 2010 DO - https://doi.org/10.1021/jf102086x SN - 0021-8561 SN - 1520-5118 VL - 58 IS - 17 SP - 9463 EP - 9467 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-21912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siegel, David A1 - Rasenko, Tatjana A1 - Koch, Matthias A1 - Nehls, Irene T1 - Determination of the Alternaria mycotoxin tenuazonic acid in cereals by high-performance liquid chromatography-electrospray ionization ion-trap multistage mass spectrometry after derivatization with 2,4-dinitrophenylhydrazine N2 - Tenuazonic acid (TA) is a major Alternaria mycotoxin. In the present work a novel approach for the detection of TA in cereals by liquid chromatography–ion-trap multistage mass spectrometry after derivatization with 2,4-dinitrophenylhydrazine is described. The product of the derivatization reaction and its major MS2 fragments were characterised by Fourier transform-ion cyclotron resonance tandem mass spectrometry. Without preconcentration, the established method features a limit of detection of 10 µg/kg using 2 g of sample in a rapid workup procedure. Accuracy, precision and linearity were evaluated in the working range of 50–5000 µg/kg. TA was detected in 13 and quantified in 3 out of 27 cereal samples obtained from a local supermarket, the average content being 49 µg/kg (highest incidence: 851 ± 41 µg/kg). KW - Tenuazonic acid KW - 2,4-Dinitrophenylhydrazine KW - Derivatization KW - Liquid chromatography-electrospray ionization ion-trap multistage mass spectrome KW - Cereals PY - 2009 DO - https://doi.org/10.1016/j.chroma.2009.03.063 SN - 0021-9673 VL - 1216 IS - 21 SP - 4582 EP - 4588 PB - Elsevier CY - Amsterdam AN - OPUS4-19382 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinsch, Martin A1 - Töpfer, Antje A1 - Lehmann, Andreas A1 - Nehls, Irene T1 - Determination of ochratoxin A in wine by liquid chromatography tandem mass spectrometry after combined anion-exchange/reversed-phase clean-up N2 - Ochratoxin A (OTA) is a mycotoxin produced by Aspergillus ochraceus and Penicillium verrucosum. It has been found and analysed in several foods and feeds. Owing to its toxicity and occurrence in food and feed, the European Community has issued directives and some countries have their own regulations for OTA contents in food, feed and beverages. This work describes a method for the determination of OTA in mulled and red wine. It is based on combined anion exchange/reversed-phase clean-up and was analysed by liquid chromatography coupled with tandem mass spectrometry (multiple reaction monitoring). The method was validated with natural contaminated and spiked wine samples with OTA contents from 1.34 to 3.48 g kg–1. Owing to its accuracy, good reproducibility and repeatability, this easy method is a good alternative to liquid chromatography–fluorescence detection methods. KW - Ochratoxin A KW - Wine KW - Tandem mass spectrometry KW - Solid-phase extraction KW - Anion exchange KW - Liquid chromatography PY - 2005 DO - https://doi.org/10.1007/s00216-005-3097-4 SN - 1618-2642 SN - 1618-2650 VL - 381 IS - 8 SP - 1592 EP - 1595 PB - Springer CY - Berlin AN - OPUS4-10306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Koch, Matthias A1 - Siegel, David A1 - Merkel, Stefan A1 - Maul, Ronald A1 - Nehls, Irene T1 - Determination of mycotoxins in foods: current state of analytical methods and limitations N2 - Mycotoxins are natural contaminants produced by a range of fungal species. Their common occurrence in food and feed poses a threat to the health of humans and animals. This threat is caused either by the direct contamination of agricultural commodities or by a "carry-over" of mycotoxins and their metabolites into animal tissues, milk, and eggs after feeding of contaminated hay or corn. As a consequence of their diverse chemical structures and varying physical properties, mycotoxins exhibit a wide range of biological effects. Individual mycotoxins can be genotoxic, mutagenic, carcinogenic, teratogenic, and oestrogenic. To protect consumer health and to reduce economic losses, surveillance and control of mycotoxins in food and feed has become a major objective for producers, regulatory authorities and researchers worldwide. However, the variety of chemical structures makes it impossible to use one single technique for mycotoxin analysis. Hence, a vast number of analytical methods has been developed and validated. The heterogeneity of food matrices combined with the demand for a fast, simultaneous and accurate determination of multiple mycotoxins creates enormous challenges for routine analysis. The most crucial issues will be discussed in this review. These are (1) the collection of representative samples, (2) the performance of classical and emerging analytical methods based on chromatographic or immunochemical techniques, (3) the validation of official methods for enforcement, and (4) the limitations and future prospects of the current methods. KW - Mycotoxins and fungal metabolites KW - Food KW - Rapid and validated methods KW - Regulations KW - Sampling KW - Multi-mycotoxin determination PY - 2010 DO - https://doi.org/10.1007/s00253-010-2535-1 SN - 0175-7598 VL - 86 IS - 6 SP - 1595 EP - 1612 PB - Springer CY - Berlin AN - OPUS4-21184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mönch, Bettina A1 - Becker, Roland A1 - Nehls, Irene T1 - Determination of ethyl glucuronide in hair: a rapid sample pretreatment involving simultaneous milling and extraction N2 - A combination of simultaneous milling and extraction known as micropulverized extraction was developed for the quantification of the alcohol marker ethyl glucuronide (EtG) in hair samples using a homogeneous reference material and a mixer mill. Best extraction results from 50 mg of hair were obtained with 2-mL plastic tubes containing two steel balls (Ø = 5 mm), 0.5 mL of water and with an oscillating frequency of 30 s-1 over a period of 30 min. EtG was quantified employing a validated GC-MS procedure involving derivatization with pentafluoropropionic acid anhydride. This micropulverization procedure was compared with dry milling followed by separate aqueous extraction and with aqueous extraction after manual cutting to millimeter-size snippets. Micropulverization yielded 28.0±1.70 pg/mg and was seen to be superior to manually cutting (23.0±0.83 pg/mg) and equivalent to dry grinding (27.7±1.71 pg/mg) with regard to completeness of EtG extraction. The option to process up to 20 samples simultaneously makes micropulverization especially valuable for the high throughput of urgent samples. KW - Ethyl glucuronide KW - Hair KW - Micropulverized extraction KW - GC-MS PY - 2014 DO - https://doi.org/10.1007/s00414-013-0939-z SN - 0937-9827 SN - 1437-1596 VL - 128 IS - 1 SP - 69 EP - 72 PB - Springer CY - Berlin ; Heidelberg AN - OPUS4-30063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ammann, Dominic A1 - Becker, Roland A1 - Kohl, Anka A1 - Hänisch, Jessica A1 - Nehls, Irene T1 - Degradation of the ethyl glucuronide content in hair by hydrogen peroxide and a non-destructive assay for oxidative hair treatment using infra-red spectroscopy N2 - The assessment of quantification results of the alcohol abuse marker ethyl glucuronide (EtG) in hair in comparison to the cut-off values for the drinking behavior may be complicated by cosmetic hair bleaching. Thus, the impact of increasing exposure to hydrogen peroxide on the EtG content of hair was investigated. Simultaneously, the change of absorbance in the range of 1000–1100 cm-1 indicative for the oxidation of cystine was investigated non-destructively by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) using pulverized portions of the respective hair samples. Hair samples treated with hydrogen peroxide consistently displayed a significantly increased absorbance at 1040 cm-1 associated with the formation of cysteic acid. The EtG content decreased significantly if the hair was treated with alkaline hydrogen peroxide as during cosmetic bleaching. It could be shown that ATR-FTIR is capable of detecting an exposure to hydrogen peroxide when still no brightening was visible and already before the EtG content deteriorated significantly. Thus, hair samples suspected of having been exposed to oxidative treatment may be checked non-destructively by a readily available technique. This assay is also possible retrospectively after EtG extraction and using archived samples. KW - Hair testing KW - Oxidation KW - Bleaching KW - Cysteic acid KW - HPLC–MS/MS PY - 2014 DO - https://doi.org/10.1016/j.forsciint.2014.07.029 SN - 0379-0738 SN - 1872-6283 VL - 244 SP - 30 EP - 35 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-31755 LA - eng 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 DO - 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 - Siegel, David A1 - Merkel, Stefan A1 - Bremser, Wolfram A1 - Koch, Matthias A1 - Nehls, Irene T1 - Degradation kinetics of the Alternaria mycotoxin tenuazonic acid in aqueous solutions N2 - The degradation kinetics of the Alternaria mycotoxin tenuazonic acid (l-TA) in aqueous buffer were studied over a period of 4 months at different pH levels (3.5 and 7.0) and temperatures (4, 25 and 40°C). l-TA and its degradation products were quantified by newly developed high-performance liquid chromatography methods with UV or electrospray multistage mass spectrometry detection. At pH 3.5, significant degradation occurred at 25 and 40°C, the respective l-TA half-lives being 73.8±0.4 and 14.0±0.1 days. Two degradation processes, epimerization and hydrolysis, were evaluated kinetically. The hydrolytically formed iso-deacetyl TA (iso-DTA, epimeric mixture) was found to be the stable end product of l-TA degradation under the conditions of this study. This indicates that iso-DTA as well as the l-TA epimer u-TA are formed in aqueous beverage matrices. KW - Tenuazonic acid KW - Alternaria KW - Epimerization KW - Degradation KW - Kinetics PY - 2010 DO - https://doi.org/10.1007/s00216-009-3288-5 SN - 1618-2642 SN - 1618-2650 VL - 397 IS - 2 SP - 453 EP - 462 PB - Springer CY - Berlin AN - OPUS4-21373 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 - Siegel, David A1 - Blaske, Franziska A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Deacetyl tenuazonic acid p-toluenesulfonylhydrazone KW - Deacetyl tenuazonic acid KW - Toluenesulfonylhydrazine KW - Hydrazone KW - Crystal structure PY - 2009 DO - https://doi.org/10.1107/S1600536809048958 SN - 1600-5368 VL - E65 IS - 12 SP - o3136 Sup-1 - o3136 Sup-8 PB - Munksgaard CY - Copenhagen AN - OPUS4-20608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siegel, David A1 - Koch, Matthias A1 - Emmerling, Franziska A1 - Nehls, Irene T1 - Deacetyl tenuazonic acid KW - Deacetyl tenuazonic acid KW - X-ray single crystal diffraction KW - Crystal structure PY - 2009 DO - https://doi.org/10.1107/S1600536809015372 SN - 1600-5368 VL - 65 IS - 6 SP - o1201 PB - Munksgaard CY - Copenhagen AN - OPUS4-19429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Das Referenzmaterial-Programm der BAM T2 - Bund-Länder-Arbeitskreis Materialprüfung CY - Berlin, Germany DA - 2000-09-27 PY - 2000 AN - OPUS4-5762 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dorgerloh, Ute A1 - Theißen, H. A1 - Becker, Roland A1 - Nehls, Irene T1 - Das Problem löst sich von selbst: Stabilisierung von Grundwasserproben zur Bestimmung organischer Inhaltsstoffe N2 - Als Folge der industriellen Produktion und der vielfältigen industriellen Nutzung von organischen Lösungsmitteln sind eine Vielzahl von Edukten, Zwischen- und Endprodukten in die Umwelt eingetragen worden und führen zu massiven Verunreinigungen des Bodens und des Grundwassers. Die Untersuchung und Sanierung des Grundwassers stellt einen aktuellen Schwerpunkt in der Altlastenbearbeitung dar. Vielfach werden klassische pump & treat-Verfahren zur Grundwassersanierung verwendet. Diese aktiven Sicherungs- und Sanierungsmaßnahmen werden jedoch unter dem Gesichtspunkt der Verhältnismäßigkeit häufig als ineffizient eingeschätzt. Als Alternative sollen die natürlichen Abbauprozesse im Grundwasserleiter genutzt oder gezielt verstärkt werden, um auf diesem Weg eine in-situ-Sanierung des Grundwasserleiters zu erreichen. In den letzten Jahren haben sich verschiedene Sanierungsverfahren etabliert, bei denen durch die Zugabe von Hilfsstoffen die mikrobiologische Aktivität des Aquifers erhöht wird bzw. Stoffe zugeführt werden, die mit den Schadstoffen reagieren (in-situ chemische Oxidation bzw. Reduktion, ISCO). An ausgewählten Standorten ist auch die aktive Sanierung (pump & treat, on-site- Sanierung) mit biologischem Schadstoffabbau (Bio-Filter) kombiniert worden. Um den Sanierungsverlauf zu verfolgen und zu optimieren, ist die Beprobung von Grundwasser aus dem Grundwasserleiter oder aus laufenden Anlagen erforderlich. In Fällen der gesteigerten mikrobiologischen Aktivität des Grundwassers treten gehäuft Probleme bei der Stabilisierung der Wasserproben auf. Die forcierten Abbauprozesse der Schadstoffe gehen nach der Probenahme in der Probenflasche weiter, bis die Energiebasis der Mikrobiologie aufgebraucht ist. Durch eine geringe Temperaturerhöhung beschleunigen sich diese Prozesse zusätzlich. In der Folge können die Schadstoffgehalte teilweise innerhalb weniger Stunden stark reduziert werden. Im Analysenlabor wird dann ein Schadstoffgehalt nachgewiesen, der nicht mehr die Verhältnisse im Aquifer bzw. im Ablauf der Reinigungsstufen widerspiegelt. Eine Einschätzung des Sanierungsfortschritts oder der Reinigungsleistung ist unter diesen Bedingungen stark fehlerbehaftet und kann zu groben Fehlinterpretationen führen. Grundwasserproben, die einem Aquifer mit hoher natürlicher oder initiierter mikrobiologischer Abbauaktivität entstammen, müssen daher zusätzlich stabilisiert werden, um den Ist-Zustand zum Zeitpunkt der Probenahme zu erfassen. Die Konservierung von Wasserproben bei der Probenahme von Grundwasser ist in der Normung umfangreich beschrieben: Die EN ISO 5667-3 von 2004 ist im Normausschuss (NA 119-01-03-01-01) überarbeitet und 2012 als Norm verabschiedet worden (EN ISO 5667-3, 03.12, deutsche Fassung DIN EN ISO 5667-3, 03-2013) [1], In Einzelfällen hat sie sich nicht als ausreichend erwiesen, um die Stabilität der organischen Schadstoffe in den oben beschriebenen Wasserproben zu gewährleisten. T2 - Altlastensymposium 2014 CY - Fulda, Germany DA - 20.03.2014 KW - Grundwasser KW - In-situ-Sanierung KW - Probenahme KW - Stabilisierung PY - 2014 SP - 76 EP - 85 AN - OPUS4-30480 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Jung, Christian A1 - Bremser, Wolfram A1 - Nehls, Irene A1 - Leschber, G. A1 - Frese, S. A1 - Walles, T. A1 - Neudecker, J. T1 - Comparison of volatile organic compounds from lung cancer patients and healthy controls—challenges and limitations of an observational study N2 - The design and operation of an observational study on the profiles of volatile organic compounds (VOC) in the breath of 37 lung cancer patients and 23 healthy controls of similar age is outlined. The necessity to quantify each VOC considered as potential disease marker on basis of individual calibration is elaborated and the quality control measures required to maintain reproducibility in breath sampling and subsequent instrumental trace VOC analysis using SPME-GC-MS over a study period of 14 months are described. 24 VOC were quantified on basis of their previously suggested potential as cancer markers. The breath concentration levels of aromatic compounds was expectedly increased in smokers while lung cancer patients displayed significantly increased levels of oxygenated VOC such as aldehydes, 2-butanone and 1-butanol. Though sets of selected oxygenated VOC displayed sensitivities and specificities between 80 and 90% using linear discriminant analysis with leave-one-out cross validation the effective selectivity of the breath VOC approach with regard to cancer detection is clearly limited. Results were discussed against the background of the literature on volatile cancer marker investigations and the prospects to link increased VOC levels in patients’ breath with approaches to employ sniffer dogs. Experiences from this study and the literature suggest that the current state of breath VOC based discrimination between cancer patients and healthy controls is hardly improvable. Observational studies tend to observe significant differences mostly in levels of certain oxygenated VOC but without resolution required for practical application. Any step towards practicable exploitation of VOC profile differences for illness detection would have to solve current restrictions set by the low and variable VOC concentrations. Further challenges are the technical complexity of studies involving breath sampling and possibly the limited capability of current analytical procedures to detect instable marker candidates. KW - Breath KW - Volatile organic compounds KW - Marker KW - Cancer KW - Gas chromatography KW - Solid phase microextraction KW - Volatilome PY - 2016 DO - https://doi.org/10.1088/1752-7155/10/4/046007 SN - 1752-7155 SN - 1752-7163 VL - 10 IS - 4 SP - Article 046007, 1 EP - 17 PB - IOP Publishing AN - OPUS4-37801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Sebastian A1 - Piechotta, Christian A1 - Godejohann, M. A1 - Win, Tin A1 - Nehls, Irene A1 - Mügge, C. T1 - Characterisation of commercially available linear alkylbenzenesulfonates by LC-SPE-NMR/MS (liquid chromatography-solid phase extraction-nuclear magnetic resonance spectroscopy-mass spectroscopy) N2 - Commercially available linear alkylbenzenesulfonates (LASs) are a mixture of various homologues and isomers, leading to 20 major species. In this work we investigated the commercial product by liquid chromatography-solid phase extraction-nuclear magnetic resonance spectroscopy-mass spectrometry (LC-SPE-NMR/MS). The commercial product was separated into 17 fractions by liquid chromatography (LC). After chromatographic separation, 5% of the flow was split to a mass spectrometer (MS) while 95% was send to post-column solid phase extraction cartridges for enrichment of the analytes (LC-SPE). After elution from the SPE-cartridges a NMR-spectrometer equipped with a cryo-probe was used for the characterisation of the different LASs species. For the first time H-1-1D and H-H-COSY spectra for 14 LASs species out of 20 major isomers are presented, whereas the 6 remaining species are detected as mixtures in 3 H-1-1D and H-H-COSY spectra. These data were used to correlate the chromatographic retention of the LASs isomers to the substitution pattern of the alkyl chain. KW - Linear alkylbenzenesulfonates KW - NMR KW - SPE KW - Liquid chromatography KW - Mass spectrometry KW - Surfactants PY - 2010 DO - https://doi.org/10.1016/j.talanta.2010.04.011 SN - 0039-9140 VL - 82 IS - 1 SP - 143 EP - 150 PB - Elsevier CY - Amsterdam AN - OPUS4-24004 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 UR - https://nbn-resolving.org/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 - JOUR A1 - Koch, Matthias A1 - Bremser, Wolfram A1 - Köppen, Robert A1 - Krüger, Rita A1 - Rasenko, Tatjana A1 - Siegel, David A1 - Nehls, Irene T1 - Certification of reference materials for ochratoxin A analysis in coffee and wine N2 - Mycotoxins are important non-anthropogenic food and feed contaminants, which can be present on almost every agricultural commodity. Effective consumer protection therefore essentially depends on food surveillance by reliable quantitative analysis enabled by appropriate quality control. Certified (matrix) reference materials (CRMs) are versatile tools to support Quality assurance. However, in the case of ochratoxin A (OTA), a hepato- and nephrotoxic mycotoxin, which is regulated in various foods, there is a lack of suitable CRMs. This lack has now been overcome by the development of two European Reference Materials (ERM®) for the Determination of OTA in roasted coffee (ERM®-BD475) and red wine (ERM®-BD476). This article discusses the material preparation process as well as the results of homogeneity and stability testing. Furthermore, the results of the inhouse certification studies carried out at BAM Federal Institute for Materials Research and Testing are presented and discussed. Interlaboratory comparison studies involving selected expert laboratories with documented Expertise in the field of mycotoxin analysis were conducted to confirm the certified values determined by BAM. The certified ochratoxin A values and their corresponding expanded uncertainties (k = 2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows: (6.0 ± 0.6) µg kg-1 for roasted coffee, ERM®-BD475, and (0.52 ± 0.11) µg L-1 for red wine, ERM®-BD476. KW - OTA KW - Coffee KW - Wine KW - Food safety and quality KW - European reference materials KW - CRM PY - 2011 DO - https://doi.org/10.1007/s00769-011-0783-0 SN - 0949-1775 SN - 1432-0517 VL - 16 SP - 429 EP - 437 PB - Springer CY - Berlin AN - OPUS4-24235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Müller-Belecke, A. A1 - Jung, Christian A1 - Nehls, Irene T1 - Bioisomerization of HBCD: Results of feeding experiments with pure Gamma-HBCD enantiomers N2 - 1,2,5,6,9,10-hexabromocyclododecane (HBCD), a widely used flame retardant, is an ubiquitous contaminant in the environment. Still, only little is known about the distribution and behavior in the environment such as bioaccumulation or biotransformation of HBCD stereoisomers. In order to investigate enrichment and possible bioisomerization of HBCD stereoisomers, Mirror Carps were exposed to pure (+)- and (-)-γ-HBCD, randomly sampled after a predefined specific period and subjected to enantiomer-specific determination of α-, β-, and γ- HBCD. No evidence for the isomerization of HBCD stereoisomers was observed in Mirror Carp fillets. T2 - Dioxin 2009 - 29th International symposium on halogenated persistent organic pollutants / Organohalogen compounds CY - Beijing, China DA - 2009-08-23 PY - 2009 UR - http://www.dioxin20xx.org/pdfs/2009/09-103.pdf VL - 71 SP - 000487 EP - 000492 CY - Beijing, China AN - OPUS4-21187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nehls, Irene A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Leschber, G. A1 - Frese, S. A1 - Neudecker, J. A1 - Walles, T. ED - Schüler, C. ED - Püschel, K. T1 - BIOAIR - Ein interdisziplinäres Projekt zur Bestimmung von Krebsmarkern in der Atemluft N2 - Wie viele Forschergruppen, haben auch wir uns das langfristige Ziel gesetzt, einen Beitrag bei der Beantwortung der Frage zu leisten, was Hunde riechen, wenn sie Krebs erschnüffeln. Dabei sollen die Hunde nicht nur anzeigen, ob eine Atemluftprobe positiv oder negativ ist, sondern sie sollen auch aktiv eingebunden werden in den systematischen Suchprozess nach detektierbaren Biomarkern. So ist geplant, dass mittels eines präparativen Fraktionssammlers definierte Schnitte des Gaschromatogramms einzeln oder in möglichen Kombinationen auf das Adsorbervlies gebracht werden, um im Hundetraining eingesetzt zu werden. In analoger Weise könnte auch mit spezifischen Kandidatensubstanzen verfahren werden. PY - 2015 SN - 978-3-8300-8763-2 N1 - Serientitel: Forschungsergebnisse aus dem Institut für Rechtsmedizin der Universität Hamburg – Series title: Forschungsergebnisse aus dem Institut für Rechtsmedizin der Universität Hamburg VL - 30 SP - 93 EP - 101 PB - Dr. Kovac AN - OPUS4-33165 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Frese, S. A1 - Leschber, G. A1 - Neudecker, J. A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Walles, T. T1 - BIOAIR - Ein interdisziplinäres Projekt zur Bestimmung von Krebsmarkern in der Atemluft T2 - 2. Symposoium Odorologie CY - Hamburg DA - 2015-03-23 PY - 2015 AN - OPUS4-32907 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Dorgerloh, Ute A1 - Win, Tin A1 - Erhardt, Ulla A1 - Hofmann, Andrea A1 - Nehls, Irene A1 - Kuhnhardt, Claus A1 - Schultze, Karin A1 - Witt, Angelika T1 - Bilanzierung der Schwefelbelastung im Grundwasser an einem ausgewählten Industriestandort, Berlin N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist vom Senat für Stadtentwicklung, Berlin, und von der Bundesanstalt für vereinigungsbedingte Sonderaufgaben (BvS) beauftragt worden, die Bilanzierung der Schwefelkomponenten für ein bis drei ausgewählte Grundwasserproben an einem Berliner Industriestandort vorzunehmen. Es handelt sich bei den Boden- und Grundwasserkontaminationen ausnahmslos um industrielle Altlasten. Da der Gehalt an organisch gebundenen Schwefelverbindungen, kolloidalem Schwefel und gelösten Sulfiden für die Dimensionierung von Grundwasseraufbereitungsanlagen (Aktivkohle, Katalysator) von großer Bedeutung ist und am Standort teilweise sehr hohe Schwefelkontaminationen auftreten, sollen vor einem erneuten Ausschreibungsverfahren zur Grundwassersanierung an drei sehr unterschiedlichen, aber für den Standort typischen Grundwassermessstellen entsprechende Bilanzen für die Schwefelbelastung erstellt werden. Dabei sind sowohl die summarischen Kenngrößen wie Summe Gesamtschwefel, ausblasbare (POS) und extrahierbare leicht- und schwerflüchtige organische Schwefelverbindungen und an Aktivkohle adsorbierbare Schwefelverbindungen (AOS) von Interesse, als auch eine Zuordnung der Hauptkontaminationen über ein halbquantitatives GC-MS-Screening. Im Artikel werden die angewendeten Verfahren vorgestellt. Die Ergebnisse werden diskutiert, gegenübergestellt und ihre Belastbarkeit eingeschätzt. T3 - BAM Forschungsberichtreihe - 265 PY - 2004 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1865 SN - 978-3-86509-182-2 SN - 0938-5533 VL - 265 SP - 1 EP - 20 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-186 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Win, Tin A1 - Schmieder, Rosemarie A1 - Erhardt, Ulla A1 - Kaminski, Katja A1 - Walther, Wolfgang A1 - Nehls, Irene T1 - Bericht zur Durchführung des Ringversuchs zur Validierung der Benzolanalytik im Spurenbereich N2 - Im Auftrag des Altlastenausschusses (ALA) der Bund/Länder Arbeitsgemeinschaft Boden (LABO) wurde ein Validierungsringversuch für die Bestimmung von leichtflüchtigen monoaromatischen Verbindungen mit Hinweisen auf existierende Prüfwerte, wie BTEX in Boden, im Spurenbereich durchgeführt. 3 Bodenproben mit unterschiedlichen Kontaminationsniveaus der BTEX-Verbindungen, überschichtet mit Methanol, eine Bodenprobe dotiert mit Ottokraftstoff, Super bleifrei, eine BTEX-Standardlösung unbekannter Konzentration, sowie eine BTEX-Standardlösung mit zertifizierten Gehaltsangaben wurden an 21 ausgewählte Teilnehmer verschickt, die überwiegend mit GC-MS analysiert haben. Die Ergebnisse und die Verfahrenskenndaten zeigen, dass die Mehrzahl der Laboratorien mit den angewandten Analysentechniken in der Lage ist, in dem vorgegebenen Kontaminationsbereich empfindlich genug, vergleichbar und richtig messen zu können. GC- FID erweist sich nicht empfindlich und spezifisch genug in dem unteren Spurenbereich, deshalb war schon in dem Aufruf zum Ringversuch auf die Anwendung der GC-MS- Messtechnik verwiesen worden. T3 - BAM Forschungsberichtreihe - 275 PY - 2006 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1769 SN - 978-3-86509-462-7 SN - 0938-5533 VL - 275 SP - 1 EP - 86 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-176 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Win, Tin A1 - Becker, Roland A1 - Lehnik-Habrink, Petra A1 - Wachholz, Sigrid T1 - BAM-zertifizierte Referenzmaterialien T2 - InCom 1999 CY - Düsseldorf, Germany DA - 1999-03-22 PY - 1999 AN - OPUS4-5813 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Lehnik-Habrink, Petra T1 - BAM CRM 5001 - Ein zertifiziertes Referenzmaterial zur Bestimmung von polychlorierten Biphenylen in Altöl T2 - 10. Jenaer Umwelttage CY - Jena, Germany DA - 1999-05-19 PY - 1999 AN - OPUS4-5715 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - BAM CRM 2001 - ein zertifiziertes Refenzmaterial zur Bestimmung von MKW in Böden T2 - 9. Jenaer Umweltanalytik-Tage 1998 CY - Jena, Germany DA - 1998-05-19 PY - 1998 AN - OPUS4-5697 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene A1 - Wachholz, Sigrid A1 - Win, Tin A1 - Lehnik-Habrink, Petra A1 - Becker, Roland T1 - BAM CRM - Tools for quality assurance in envirinmental analysis T2 - 37th IUPAC Congress CY - Berlin, Germany DA - 1999-08-14 PY - 1999 AN - OPUS4-5815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maul, Ronald A1 - Kittler, Katrin A1 - Koch, Matthias A1 - Nehls, Irene T1 - Bakterielle Migranten - Algentoxine als neue Herausforderung in der Umweltanalytik N2 - Bioaktive Sekundärstoffe aus Cyanobakterien stellen eine Quelle für pharmazeutisch interessante Wirkstoffkandidaten wie auch eine Herausforderung für die Umwelt- und Lebensmittelanalytik dar. Die Identifizierung ist allerdings nicht trivial. KW - Cyanotoxine KW - Analytik PY - 2011 SN - 0344-1733 SN - 1610-8256 IS - August SP - 56 EP - 58 PB - Vogel CY - Würzburg AN - OPUS4-25733 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 - Aufgaben der BAM - Referenzmaterialien T2 - Veranstaltung der SEPAWA CY - Berlin, BAM, Deutschland DA - 2000-09-08 PY - 2000 AN - OPUS4-959 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehls, Irene T1 - Aufgaben der BAM - Referenzmaterialien T2 - Veranstaltung der SEPTAWA in der BAM CY - Berlin, Germany DA - 2000-09-08 PY - 2000 AN - OPUS4-5761 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 - Nehls, Irene T1 - Analytik von Mineralölen - Standards für die Kohlenwasserstoff-Analytik KW - Kalibrierstandard KW - Diesel KW - Schmieröl KW - Kohlenwasserstoffe KW - GC-FID PY - 2006 SN - 0016-3538 VL - 50 IS - 4 SP - 290 EP - 291 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-12280 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 DO - 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 - 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 - TY - JOUR A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Nehls, Irene A1 - Becker, Roland T1 - A Proof of Concept: Are Detection Dogs a Useful Tool to Verify Potential Biomarkers for Lung Cancer? N2 - Early and reliable diagnostic test is essential for effective therapy of lung cancer. Volatile organic compounds that are characteristic for cancer could serve as valuable biomarkers in cancer diagnosis. Both trace analytical and detection dog approaches give some evidence for the existence of such biomarkers. In this proof of concept, study dogs and trace analysis were implemented in combination to gain more information concerning cancer biomarkers. Two dogs were trained to distinguish between absorbed breath samples of lung cancer patients and healthy persons and succeeded with correct identification of patients with 9/9 and 8/9 and correct negative indications from of 8/10 and 4/10 samples from healthy individuals. A recent observational study found that breath samples from lung cancer patients showed an increase in 1-butanol, 2-butanone, 2-pentanone, and hexanal. Synthetic air samples were therefore fortified with these compounds and adsorbed to a fleece. Tested against breath samples from healthy probands, on presentation to the dogs these synthetic samples provoked an indication in three out of four samples. We were able to demonstrate that a combination of the natural nose of a dog and a trace analytic technique can be a valuable concept in the search for cancer biomarkers. KW - Lung cancer KW - Breath KW - Detection dog KW - Biomarkers KW - Sampling KW - Synthetic air PY - 2018 DO - https://doi.org/10.3389/fvets.2018.00052 SN - 2297-1769 VL - 5 SP - Article 52,1 EP - 6 PB - Frontiers Research Foundation CY - Lausanne AN - OPUS4-44466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neuhof, Torsten A1 - Ganzauer, Natalie A1 - Koch, Matthias A1 - Nehls, Irene T1 - A comparison of chromatographic methods for the determination of deoxynivalenol in wheat N2 - Liquid chromatography coupled with tandem mass spectrometric detection has gained more importance for mycotoxin determination in recent years. In addition to instrumental improvements, the development of LC-MS-MS has also been a consequence of the availability of stable isotope internal standards, e.g., 13C-labelled mycotoxins. Thus, the LC-ESI-MS-MS method using a 13C15-deoxynivalenol internal standard as a state-of-the-art technique was selected as a reference procedure for an in-house method comparison study of the determination of deoxynivalenol (DON) in wheat materials. Alternative methods include LC-diode array detection, which is a frequently used routine procedure for DON-analysis, and gas chromatography after trimethylsilylation. For GC application, an electron capture detector and a negative chemical ionisation mass spectrometry detector were used, which have both been well described in the literature. The method comparison was conducted using t test statistics. Additionally, this study also calculates important method performance characteristics, including accuracy, linearity, limit of detection, limit of quantification, recovery, and variation coefficient. Furthermore, this is the first report of a GC-MS method for the determination of DON using a fully carbon-labelled 13C15-DON as an IS. The GC-MS using 13C15-DON as an IS has produced comparable results to the 13C-IS-LC-MS-MS reference method with a similar sensitivity. ECD detection was slightly less sensitive, but is also suited for DON analysis in wheat. Due to the high LOQ, the LC-DAD method seems highly applicable to the measurement of highly contaminated samples. KW - Column liquid chromatography-mass spectrometry KW - Gas chromatography KW - Mycotoxins KW - Trichothecenes PY - 2009 DO - https://doi.org/10.1365/s10337-009-1084-1 SN - 0009-5893 SN - 1612-1112 VL - 69 IS - 11-12 SP - 1457 EP - 1462 PB - Vieweg CY - Wiesbaden AN - OPUS4-19618 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 - JOUR A1 - Kuhlich, Paul A1 - Göstl, Robert A1 - Metzinger, R. A1 - Piechotta, Christian A1 - Nehls, Irene T1 - 3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetrahydro-2-naphthoic acid (AHTN-COOH) KW - AHTN KW - Tonalide KW - Cyclilc musk KW - AHTN-COOH KW - Disinfection by-product KW - Haloform reaction PY - 2010 DO - https://doi.org/10.1107/S1600536810038572 SN - 1600-5368 VL - 66 IS - 10 SP - o2687, sup-1 - sup-12 PB - Munksgaard CY - Copenhagen AN - OPUS4-23006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -