TY - CONF A1 - Schreiner, M. A1 - Krumbein, A. A1 - Rohn, S. A1 - Kittler, Katrin A1 - Hoffmann, H. A1 - Koch, Matthias A1 - Maul, Ronald T1 - Entwicklung eines HPLC-MS/MS basierten Isotopenverdünnungsverfahrens zur Quantifizierung des Cyanotoxins Cylindrospermopsin in Brassica-Arten T2 - Deutscher Lebensmittelchemikertag CY - Berlin, Germany DA - 2013-09-16 PY - 2013 AN - OPUS4-29127 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schreiner, M. A1 - Krumbein, A. A1 - Rohn, S. A1 - Kittler, Katrin A1 - Hoffmann, Holger A1 - Koch, Matthias A1 - Maul, Ronald T1 - Enhanced LC-MS/MS-Analysis of Cylindrospermopsin in Plant and Freshwater Matrices Using the Stable Isotope Dilution Assay T2 - RAFA 2013 CY - Prague, Czech Republic DA - 2013-11-05 PY - 2013 AN - OPUS4-29484 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schreiner, M. A1 - Krumbein, A. A1 - Manzei, St. A1 - Rohn, S. A1 - Kittler, Katrin A1 - Koch, Matthias A1 - Maul, Ronald T1 - Nachweis der Resorption des Cyanotoxins Cylindrospermopsin durch Brassica-Arten T2 - Deutscher Lebensmittelchemikertag 2012 CY - Münster, Germany DA - 2012-09-10 PY - 2012 AN - OPUS4-26494 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schloß, Svenja A1 - Wedell, Ines A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, Ronald T1 - Biosynthesis and characterization of 15N6-labeled phomopsin A, a lupin associated mycotoxin produced by Diaporthe toxica N2 - The hepatotoxin phomopsin A (PHO-A), a secondary metabolite mainly produced by the fungus Diaporthe toxica, occurs predominantly on sweet lupins. Along with the growing interest in sweet lupins for food and feed commodities, concerns have been raised about fungal infestations, and consequently, about the determination of PHO-A. High performance liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) represents the most suitable analytical technique for sensitive and selective detection of mycotoxins including PHO-A. However, isotopic labeled substances are needed as internal standards for a reliable and convenient quantification. As no isotope standard for PHO-A is currently available, a biosynthesis of fully 15N6-labeled PHO-A was established by cultivation of D. toxica on defined media containing Na15NO3 and 15N-labeled yeast extract as the only nitrogen sources. The identity of 15N6-PHO-A was confirmed by high resolution mass spectrometry. The new 15N6-labeled standard will facilitate the method development for PHO-A including a more accurate quantification by LC-MS/MS. KW - Phomopsin A KW - Lupins KW - Diaporthe toxica KW - Stable isotope dilution assay KW - Isotopic labeled internal standard KW - Biosynthesis PY - 2015 U6 - https://doi.org/10.1016/j.foodchem.2014.12.056 SN - 0308-8146 VL - 177 SP - 61 EP - 65 PB - Elsevier CY - Amsterdam [u.a.] ; Jena AN - OPUS4-32464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schloß, Svenja A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, R. T1 - Development of a SIDA-LC-MS/MS method for the determination of phomopsin A in legumes N2 - A novel method for the determination of phomopsin A (1) in lupin flour, pea flour, and bean flour as well as whole lupin plants was established based on stable isotope dilution assay (SIDA) LC-MS/MS using 15N6-1 as an isotopically labeled internal standard. Artificially infected samples were used to develop an optimized extraction procedure and sample pretreatment. The limits of detection were 0.5–1 µg/kg for all matrices. The limits of quantitation were 2–4 µg/kg. The method was used to analyze flour samples generated from selected legume seeds and lupin plant samples that had been inoculated with Diaporthe toxica and two further fungal strains. Finally, growing lupin plants infected with D. toxica were investigated to simulate a naturally in-field mycotoxicosis. Toxin levels of up to 10.1 µg/kg of 1 were found in the pods and 7.2 µg/kg in the stems and leaves. KW - Diaporthe toxica KW - Stable isotope dilution assay KW - Isotopic labeled internal standard KW - Legume contamination PY - 2015 U6 - https://doi.org/10.1021/acs.jafc.5b04792 SN - 0021-8561 SN - 1520-5118 VL - 63 IS - 48 SP - 10543 EP - 10549 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-35071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schloß, S. A1 - Hackl, T. A1 - Herz, C. A1 - Lamy, E. A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, R. T1 - Detection of a Toxic Methylated Derivative of Phomopsin A Produced by the Legume-Infesting Fungus Dioporthe toxica N2 - Phomopsin A (PHO-A), produced by the fungus Diaporthe toxica, is a mycotoxin known to be responsible for fatal liver disease of lupin-fed sheep. The füll spectrum of the toxic secondary metabolites produced by D. toxica is still unknown. PHO-A and the naturally occurring derivatives B—E have been subject to several studies to reveal their structures as well as chemical and toxicological properties. In this work, a methylated derivative of PHO-Aisolated firom lupin seeds inoculated %vith D. toxica is described. It was characterized by high-resolution mass and NMR data and shown to be the N-methylated derivative of PHO-A 1 is cytotoxic againstHepG2 cells. KW - Mycotoxins KW - Identification KW - Food PY - 2017 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-411167 VL - 80 IS - 6 SP - 1930 EP - 1934 PB - ACS Publications AN - OPUS4-41116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kittler, Katrin A1 - Schreiner, M. A1 - Krumbein, A. A1 - Rohn, S. A1 - Koch, Matthias A1 - Maul, Ronald T1 - Resorption des Cyanotoxins Cylindrospermopsin durch Brassica-Arten T2 - Regionalverbandstagung Nordost CY - Berlin, Germany DA - 2013-03-14 PY - 2013 AN - OPUS4-27832 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kittler, Katrin A1 - Schreiner, M. A1 - Krumbein, A. A1 - Rohn, S. A1 - Koch, Matthias A1 - Maul, Ronald T1 - Detection of the Cyanotoxin Cylindrospermopsin in Brassica Species T2 - JCF Frühjahrssymposium CY - Berlin, Germany DA - 2013-03-06 PY - 2013 AN - OPUS4-27833 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittler, Katrin A1 - Schreiner, M. A1 - Krumbein, A. A1 - Manzei, S. A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, Ronald T1 - Uptake of the cyanobacterial toxin cylindrospermopsin in brassica vegetables N2 - Toxin-producing cyanobacterial species are increasingly being found in freshwater systems. However, literature on the impact of many cyanobacterial toxins on plants is scarce. Cylindrospermosin (CYN), a secondary metabolite of cyanobacteria such as Cylindrospermopsis and Aphanizomenon species, is a potent hepatotoxin and protein synthesis inhibitor. Worryingly, CYN is increasingly found in surface and drinking water worldwide causing human and animal intoxications. Further, exposure of crop plants to CYN by irrigation with contaminated water has already been shown. Therefore, in this study, horticulturally important and highly consumed Brassica species were investigated to determine the level of CYN in the leaves after exposure of the roots to the toxin. Treatment of Brassica oleracea var. sabellica, Brassica juncea, and Sinapis alba under varying experimental conditions showed significant CYN uptake, with CYN levels ranging from 10% to 21% in the leaves compared to the CYN concentration applied to the roots (18–35 µg/l). In seedlings, CYN concentrations of up to 49 µg/g fresh weight were observed. Thus, crop plants irrigated with CYN-containing water may represent a significant source of this toxin within the food chain. KW - Cylindrospermopsin KW - Plant systemic availability KW - Cyanobacterial toxin KW - Brassicaceae KW - Exposure source PY - 2012 U6 - https://doi.org/10.1016/j.foodchem.2012.01.107 SN - 0308-8146 VL - 133 IS - 3 SP - 875 EP - 879 PB - Elsevier CY - Amsterdam [u.a.] ; Jena AN - OPUS4-25730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittler, Katrin A1 - Hoffmann, Holger A1 - Lindemann, Franziska A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, Ronald T1 - Biosynthesis of 15N-labeled cylindrospermopsin and its application as internal standard in stable isotope dilution analysis N2 - Cylindrospermopsin (CYN) is a cyanobacterial toxin associated with human and animal poisonings. Due to its toxicity in combination with its widespread occurrence, the development of reliable methods for selective, sensitive detection and accurate quantification is mandatory. Liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis using stable isotope dilution analysis (SIDA) represents an ideal tool for this purpose. U-[15N5]-CYN was synthesized by culturing Aphanizomenon flos-aquae in Na15NO3-containing cyanobacteria growth medium followed by a cleanup using graphitized carbon black columns and mass spectrometric characterization. Subsequently, a SIDA-LC-MS/MS method for the quantification of CYN in freshwater and Brassica matrices was developed showing satisfactory performance data. The recovery ranged between 98 and 103 %; the limit of quantification was 15 ng/L in freshwater and 50 µg/kg dry weight in Brassica samples. The novel SIDA was applied for CYN determination in real freshwater samples as well as in kale and in vegetable mustard exposed to toxin-containing irrigation water. Two of the freshwater samples taken from German lakes were found to be CYN-contaminated above limit of quantification (17.9 and 60.8 ng/L). CYN is systemically available to the examined vegetable species after exposure of the rootstock leading to CYN mass fractions in kale and vegetable mustard leaves of 15.0 µg/kg fresh weight and 23.9 µg/kg fresh weight, respectively. CYN measurements in both matrices are exemplary for the versatile applicability of the developed method in environmental analysis. KW - Cyanotoxin KW - Quantification KW - Surface water KW - Vegetable plants KW - SIDA KW - HPLC-MS/MS PY - 2014 U6 - https://doi.org/10.1007/s00216-014-8026-y SN - 1618-2642 SN - 1618-2650 VL - 406 IS - 24 SP - 5765 EP - 5774 PB - Springer CY - Berlin AN - OPUS4-31566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -