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 -