For the Fusarium trichothecene mycotoxins T-2 and HT-2, a combined (T-2 + HT-2) temporary tolerable daily intake (tTDI) of 0.06 microg kg(-1) body weight day(-1) was proposed at the European level in 2001 (Opinion of the Scientific Committee on Food). In the near future, maximum levels for these trichothecenes will be regulated by the European Commission as announced in EU (VO) 1881/2006. For the implementation of these maximum levels, more data on occurrence and behaviour of T-2 and HT-2 toxins in primary agricultural products as well as during cleaning treatment and food processing are needed. In the current work, we determined the T-2/HT-2 concentrations in four oat cultivars (Aragon, Dominik, Ivory, Pergamon) from ten different agricultural sites in Germany, grown in cultivar studies in 2007. The grains were de-hulled, oat meal was prepared, and bread with 20% oat meal and 80% wheat flour was baked. In the cereal-processing chain, samples were taken at various steps and subsequently analysed for their T-2/HT-2 content. We employed liquid chromatography-mass spectrometry (LC-MS) and an immunological screening method (enzyme-linked immunoabsorbent assay (ELISA)) for T-2/HT-2 determination. Detection limits were between 1 and 10 microg kg(-1) in different matrices. T-2/HT-2 concentrations determined by ELISA in oat samples from ten different agricultural sites in Germany were between 9 and 623 microg kg(-1). The median and 90th percentile were 48 and 191 microg kg(-1) T-2/HT-2, respectively. One site showed six times higher T-2/HT-2 levels than the other sites, where concentrations ranged from 322 to 623 microg kg(-1). In 80% of the samples the cultivars Pergamon and Ivory had the lowest concentration of T-2 and HT-2 toxins. Using LC-MS for T-2/HT-2 determination, cleaning of the raw material did not lead to significant reductions of T-2 and HT-2 levels, whereas de-hulling led to a reduction of over 90%. Boiling of oat meal produced from cleaned raw material to yield 'porridge' resulted in varying T-2/HT-2 levels in experimental replicates. No major reduction of T-2/HT-2 levels in cooked porridge was obtained. Standardized baking experiments using 20% oat meal showed that T-2 and HT-2 toxins are relatively stable during the baking process, probably due to their temperature stability.

Mycotoxins are among the most abundant contaminants in food and feed worldwide. Therefore, in the EU maximum levels are established, e.g. for the frequently occurring Fusarium toxins deoxynivalenol (DON) and zearalenone (ZEA). Additional to DON and ZEA, modified mycotoxins are present in naturally contaminated grain products contributing significantly to the exposure of humans and animals with mycotoxins. Up to now data on the spatial distribution of many (masked) mycotoxins in the kernels of wheat are missing. The aim of the present study was to investigate the amounts of DON and ZEA as well as their most abundant derivatives DON-3-glucoside (DON-3G), 3- and 15-acetyl-DON, ZEA-14- and 16-glucoside and ZEA-14-sulphate (ZEA-14S) in mill fractions of naturally contaminated wheat batches using HPLC-MS/MS. The investigated distribution pattern in ten milling fractions is comparable among the three investigated different wheat batches. Interestingly, DON and DON-3G were found to be present to similar amounts in all fractions. In bran, the levels were only slightly higher than in the endosperm. By contrast, for ZEA and ZEA-14S a significantly higher amount of toxin is located in the fibre-rich fractions. The relative mass proportion of DON-3G comprises for only between 2.9 and 11.2% of the free DON, while the relative mass proportion of ZEA-14S is estimated to even exceed the amount of free ZEA in certain fractions. Acetylated DON derivatives and ZEA-glucosides were only detected in low amounts. The experimental results show that a significant reduction of the ZEA and ZEA-14S level in wheat flour is feasible by applying milling technology strategies. However, the almost evenly distribution of DON and DON-3G in all fractions does not allow for the technological removal of relevant toxin amounts. Furthermore, the relative share of masked forms was higher for ZEA derivatives than for the DON conjugates in the investigated wheat lots.

Abkürzungen: anhydro-CTC = Anhydrochlortetracyclin; BFEL = Bundesforschungsanstalt für Ernährung und Lebensmittel; BG = Bestimmungsgrenze; CTC = Chlortetracyclin; EDTA = Ethylendiamintetraacetic acid; enol-epi-CTC = Enolform des epiChlortetracyclins; epi-CTC = epi-Chlortetracyclin; epi-iso-CTC = epi-Isochlortetracyclin; ESI = Electrospray Ionisation; FAL = Bundesforschungsanstalt für Landwirtschaft; FEDESA = Federation Européenne de la Santé Animale; FG = Frischgewicht; HPLC = High Performance Liquid Chromatography; iso-CTC = Isochlortetra cyclin; ISTD = interner Standard; KGW = Körperge-wicht; keto-epi-CTC = Ketoform des epi-Chlortetracyclins; LC-MS/ MS = Flüssigchromatographie / Tandem-Massenspektrometrie; LEJ = Landesamt für Ernährungswirtschaft und Jagd; MS = Massenspektrometrie; MS 2 = Tandem-Massenspektrometrie; MRL = Maximum Residue Limit; MHK = Minimale Hemmstoffkonzentration; MUNLV = Ministerium für Umwelt und Naturschutz, Landwirtschaft und Verbraucherschutz des Landes Nordrhein-Westfalen; n = Anzahl der Messwerte; N4-SFD = N4-Acetylsulfadiazin; N/F = nicht nachgewiesen (not found); NWG = Nachweisgrenze; OTC = Oxytetracyclin; PDA = Photodiodenarraydetektor / detektion; PAK = polycyclische aromatische Kohlenwasserstoffe; PCB = polychlorierte Biphenyle; SFD = Sulfadiazin; SPE = Solid Phase Extraction; SRM = Selective Reaction Monitoring; TC = Tetracyclin; TIC = Totalionenstrom; TM = Trockenmasse; TMP = Trimethoprim; UFT = Zentrum für Umweltforschung und Umwelttechnologie, Universität Bremen; W = Wiederfi ndung. Zusammenfassung: In einem Modellversuch wurde unter praxisnahen landwirtschaftlichen Bedingungen untersucht, ob Nutzpfl anzen Antibiotika aus Böden aufnehmen, die zuvor mit belasteter Gülle gedüngt worden sind. Dazu wurden Ferkel mit Sulfadiazin (SFD), Trimethoprim (TMP) und Chlortetracyclin (CTC) oral medikamentiert, um kontrolliert Arzneistoff-belastete Schweinegülle zu erhalten. Die Gülle aus 2 Medikationen wurde ca. 8 Monate gelagert und dann zur Düngung der Aussaat von Feldsalat und Winterweizen auf Versuchsparzellen ausgebracht.Während der Lagerung waren CTC und SFD nur bis zu 50-60% abbaubar, daher wurden auf die Felder z.T. erhebliche Antibiotikafrachten ausgetragen (176-284 mg CTC/m 2 und 557-922 mg SFD/m 2 ). Bodenproben wurden in unterschiedlichen Horizonten sowie Pfl anzenproben in verschiedenen Wachstumsstadien bis zur Beerntung genommen und analysiert. In Extrakten der oberen Bodenhorizonte (0-25 cm), die nach der ersten Güllebe-aufschlagung der Versuchsfelder beprobt wurden, sind SFD (90 g/kg TM) und CTC (bestimmt als iso-/epi-iso-CTC-Summenparameter: max. 240 g/kg TM) nachgewiesen worden, aber nicht in tieferen Schichten bis zu 60 cm. In Parzellen, die zweimal organisch gedüngt worden waren, traten die höchsten Belastungen auf. Nach 3 Monaten lagen nur noch Antibiotikagehalte von ca. 10-20 g/kg TM vor.Feldsalat und Winterweizen haben aus den organisch gedüngten Böden Antibiotika über die Wurzel aufgenommen. Bei den Getreidepfl anzen war die zeitliche Veränderung der SFD/ CTC-Gehalte...

Feedingstuffs are frequently contaminated with sclerotia (ergot) of the phytopathogenic fungus Claviceps purpurea. Ergot contains ergot alkaloids (EA), but the amount and composition of these substances may be highly variable hampering the extrapolation of the amount of EA from the ergot content. 600 different feed samples from the harvest years 2011–2014 (rye, triticale, wheat, mixed cereal grains or compound feed), preferably those with visible ergot infestation, were analyzed for both parameters ergot and EA content in a German monitoring program. The analytical results were employed for statistical evaluation using the software JMP® 13. The data show that the correlation between the ergot and the EA content was rather poor, especially for rye, the grain most frequently contaminated with ergot and EA. Consequently, effects on animal health correlated much better with EA than with ergot content. Furthermore, it shows that the current European law for undesirable substances (Directive 2002/32/EC) restricting the ergot content in feed materials and compound feed containing unground cereals is not fully sufficient to protect animal health. Therefore, preliminary guidance values for species-specific critical values for total EA content in the diets are derived and suggested for practical use. Further research is needed to verify these preliminary guidance values and to improve risk evaluation in consideration of the significant variability in the species-specific sensitivity.

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Concentrations of tetracyclines found in wheat and rye grains were of no concern with respect to toxicity regarding human consumption. However, antibiotic concentrations below the minimum inhibitory concentration can select for antibiotic resistance in bacteria. Thus, low levels of different tetracycline residues contained in food should be taken into account regarding risk assessment. © 2018 Society of Chemical Industry.

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