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Pyrrolizidine alkaloids (PAs) are secondary metabolites of plant families such as Asteraceae or Boraginaceae and are suspected to be genotoxic carcinogens. Recent investigations revealed their frequent occurrence in honey and particularly in tea. To obtain a comprehensive overview of the PA content in animal- and plant-derived food from the European market, and to provide a basis for future risk analysis, a total of 1105 samples were collected in 2014 and 2015. These comprised milk and milk products, eggs, meat and meat products, (herbal) teas, and (herbal) food supplements collected in supermarkets, retail shops, and via the internet. PAs were detected in a large proportion of plant-derived foods: 91% of the (herbal) teas and 60% of the food supplements contained at least one individual PA. All types of (herbal) teas investigated were found to contain PAs, with a mean concentration of 460 µg kg−1 dry tea (corresponding to 6.13 µg L−1 in [herbal] tea infusion). The highest mean concentrations were found in rooibos tea (599 µg kg−1 dry tea, 7.99 µg L−1 tea infusion) and the lowest in camomile tea (274 µg kg−1 dry tea, 3.65 µg L−1 tea infusion). Occurrence of PAs in food supplements was found to be highly variable, but in comparable ranges as for (herbal) tea. The highest concentrations were present in supplements containing plant material from known PA-producing plants. In contrast, only 2% of the animal-derived products, in particular 6% of milk samples and 1% of egg samples, contained PAs. Determined levels in milk were relatively low, ranged between 0.05 and 0.17 µg L−1 and only trace amounts of 0.10–0.12 µg kg−1 were found in eggs. No PAs were detected in the other animal-derived products.

Kokzidiostatika werden in der Kleintiermast als Futtermittelzusatzstoffe zur Vorbeugung der Kokzidiose eingesetzt. Die Verwendung der Wirkstoffe ist in der Europäischen Union gesetzlich geregelt und unterliegt der amtlichen Lebens- und Futtermittelkontrolle. In der vorliegenden Arbeit wurden Methoden zur flüssigchromatographisch tandem-massen¬spektro¬metrischen (LC-MS/MS-) Bestimmung von Kokzidiostatika in Futtermitteln und in Ei entwickelt. Durch Bestandteile des Probenmaterials traten Störungen des Analytsignals auf. Die Untersuchung solcher Matrixeffekte ist in der pharmazeutischen und der Pestizidanalytik üblich. Zu Matrixeffekten bei der LC-MS/MS-Analytik in Futtermitteln gibt es kaum Daten. Ein Schwerpunkt dieser Arbeit war daher die Untersuchung der Einflussfaktoren auf Matrixeffekte bei der Analyse von Kokzidiostatika. Aufgrund der gewonnenen Erkenntnisse wurde eine Methode zur Bestimmung von Verschleppungen von Kokzidiostatika in Futtermittel für Nichtzieltierarten entwickelt und validiert. Weitere LC-MS/MS-Methoden wurden zur Bestimmung Maduramicins in Futtermittel, Eiweiß und Eigelb optimiert. Diese wurden zur wurden zur Untersuchung des Übergangs des Kokzidiostatikums aus dem Futtermittel in das Ei benötigt. Dazu wurde eine Fütterungsstudie mit Legehennen durchgeführt. Futtermittel mit drei Konzentrationen von Maduramicin bis zum Höchstgehalt in Futtermittel für Nichtzieltierarten wurden hergestellt und je einer Gruppe von Legehennen verabreicht. Das aufgenommene Maduramicin ging ausschließlich ins Eigelb über, es ergab sich eine Carry-over-Rate von 8 %. Der für Eier festgelegte Höchstgehalt von 2 µg/kg wurde überschritten, obwohl die Konzentrationen Maduramicins in den verfütterten Futtermitteln unterhalb des Höchstgehaltes für Futtermittel lagen. Als Folge dieser Ergebnisse wurde der Maduramicin-Höchstgehalt in Ei auf 12 µg/kg angepasst. Der in Verordnung (EG) Nr. 124/2009 festgelegte Höchstgehalt wurde durch die Verordnung (EU) 610/2012 geändert., Prevention of coccidosis by anticoccidial feed additives is of great economic importance in poultry farming. Application of these substances is regulated by European law and is a matter of official feed and food control requiring appropriate determination methods for coccidiostats. In this study, liquid chromatographic tandem mass spectrometric (LC-MS/MS-) methods for the quantification of coccidiostats in feed and eggs were developed. The influence of the sample material resulted in poor method performance. These matrix effects are intensively investigated in other analytical fields like drug or pesticide analysis. In contrast, there are limited data concerning matrix effects in LC-MS/MS analysis in feedingstuffs. This study therefore focussed on the systematic investigation of factors influencing matrix effects during analysis of coccidiostats. The findings were implemented in the development and validation of a method for the determination of cross-contamination levels of authorized coccidiostats in feed for non-target animals. This method was optimized for the determination of the anticoccidial feed additive maduramicin in feed, egg white, and egg yolk for a carry-over study. By means of the conducted feeding trial with laying hens the carry-over of maduramicin from feed into eggs was comprehensively characterized. Three feedingstuffs containing different levels of maduramicin up to the maximum tolerable level in non-target animal feed were prepared and fed to groups of ten laying hens. Maduramicin is exclusively transferred into egg yolk, and a carry-over rate into whole eggs of 8 % was calculated. Although the applied diets were in compliance with the maximum level in feed, resulting concentrations in whole eggs exceeded the maximum level in eggs. As a consequence of these findings, the maximum permitted level of maduramicin in eggs was adapted to 12 µg/kg. The maximum level assigned by Regulation (EC) No. 124/2009 was amended in Regulation (EU) 610/2012.