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.

Le aflatossine sono potenti sostanze cancerogene presenti in natura. L'aflatossina b1 viene poco degradata nel rumine ed è escreta nel latte come aflatossina M1 con un carry over del 1-3%. Nel presente lavoro è stata studiata l'apparizione delle aflatossine nel sangue conseguente all'ingestione orale di un bolo contaminato per verificare come queste tossine sono assorbite nel tratto digestivo delle vacche da latte. La comparsa nel plasma e nel latte attraverso una mucosa tipicamente non di assorbimento per determinare il possibile meccanismo che regola l'assorbimento delle aflatossine è stato un ulteriore oggetto di studio. Un'altra prova è stata effettuata con vacche da latte per studiare il carry-over dell'aflatossina B1 nel latte in relazione al livello produttivo e alle cellule somatiche, come indicatore di processi infiammatori nella mammella. La capacità sequestrante di diversi tipi di adsorbenti è stata comparata in prove in vitro condotte in differenti condizioni sperimentali. Anche il comportamento del complesso aflattosina-adsorbente nel tratto digestivo di vacche in lattazione è stato studiato in vivo per mezzo della misurazione della presenza di aflatossina M1 nel latte. Una prova in vivo è stata effettuata per verificare l'effetto che la pellettatura o la semplice miscelazione di adsorbenti nei mangimi può avere nel migliorare l'efficienza di sequestro. / Aflatoxins are the most potent natural carcinogenic compound present in nature. Aflatoxin B1 is poorly degraded in the rumen and is excreted in milk as aflatoxin M1 with a carry-over rate of 1-3%. The present work investigated rate and schedule of aflatoxins plasma appearance following an oral contaminated bolus to verify how these toxins are absorbed in the gastro-intestinal tract of dairy cows. Aflatoxins plasma and milk appearances were also investigated using a non-absorbing mucosa to understand the possible aflatoxins absorption mechanism through mucous membranes. A trial was carried out in lactating dairy cows to study the carry over of ingested aflatoxin B1 in milk as aflatoxin M1 in relation to milk yield and somatic cells count, the latter as indicator of udder inflammatory processes. sequestering capacity of different kinds of mycotoxins sequestering agents were compared in vitro trial carried out at different experimental conditions. The behaviour of the aflatoxins-adsorbents complexes through digestive tract of lactating dairy cows were also investigated in vivo by measuring appearance of aflatoxin M1 into milk. An in vivo trial was conducted to verify if effect of pelletizing or simply mixing processes is useful to improve mycotoxins sequestering agents efficacy in dairy cow nutrition.

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Submitted by JÚLIO HEBER SILVA (julioheber@yahoo.com.br) on 2018-06-11T19:53:05Z No. of bitstreams: 2 Dissertação - Cássia Cardoso de Carvalho Vasconcelos - 2018.pdf: 1013495 bytes, checksum: 354b152bc79c9682f78ed5fbe130c19e (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Rejected by Luciana Ferreira (lucgeral@gmail.com), reason: Olhei nas dissertações que já foram inseridas para checar a citação, veja como deve ser: Ex.: Dissertação (Mestrado em Administração Pública em Rede Nacional) - on 2018-06-12T12:17:16Z (GMT) / Submitted by JÚLIO HEBER SILVA (julioheber@yahoo.com.br) on 2018-06-12T16:49:51Z No. of bitstreams: 2 Dissertação - Cássia Cardoso de Carvalho Vasconcelos - 2018.pdf: 1013495 bytes, checksum: 354b152bc79c9682f78ed5fbe130c19e (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2018-06-13T10:41:33Z (GMT) No. of bitstreams: 2 Dissertação - Cássia Cardoso de Carvalho Vasconcelos - 2018.pdf: 1013495 bytes, checksum: 354b152bc79c9682f78ed5fbe130c19e (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Made available in DSpace on 2018-06-13T10:41:33Z (GMT). No. of bitstreams: 2 Dissertação - Cássia Cardoso de Carvalho Vasconcelos - 2018.pdf: 1013495 bytes, checksum: 354b152bc79c9682f78ed5fbe130c19e (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Previous issue date: 2018-06-08 / The object of study of this research is expenses classified as carryovers, which are part of the public budget, and they are a challenge for public managers. The objective of the research is to propose a control instrument applicable to the budgetary and financial execution of an IFES, considering the legislation applicable to the public budget, that assists the manager in controlling and reducing the effects of expenses classified as carryovers. Descriptive analysis and application of Pearson's correlation index were carried out on data taken from the Federal Government's Portal, referring to the five universities in the Center-West region between 2008 and 2016. It is concluded that: carryovers are present in all universities evaluated; on average, more than a quarter of the budget started is not finalized in the same year; unprocessed leftovers account for more than 90% of the total unpaid debts of universities. Furthermore, it is found that: there is a moderate negative correlation to budget execution and unbundling of UNB; there is a moderate positive correlation between the remainders to be paid and the financial execution of the budget in the UFGD and the UNB, and negative correlation in the UFG. The intervention proposal has two stages: the first one is the collection of information on the budgetary and financial situation of IFES, through a control sheet, and the second step is the application of the GUT matrix in the budget balances of the carryovers, to prioritize the closure of such expenses. / O objeto desta pesquisa são as despesas classificadas como restos a pagar, que fazem parte da execução do orçamento público, e se apresentam como um desafio para os gestores públicos. O objetivo da pesquisa é propor um instrumento de controle aplicável à execução orçamentária e financeira de uma IFES, considerando a legislação aplicável ao orçamento público, que auxilie o gestor no controle e na redução dos efeitos das despesas classificadas como restos a pagar. Por meio da análise descritiva e aplicação do índice de correlação de Pearson de dados retirados do Portal Siga Brasil referentes às cinco universidades da região Centro-Oeste, entre os anos de 2008 e 2016, conclui-se que: os restos a pagar estão presentes em todas as universidades avaliadas; em média, mais de um quarto do orçamento iniciado não é finalizado no mesmo exercício; os restos a pagar não processados representam, em média, mais de 90% dos restos a pagar total das universidades, e constatou-se que: há correlação moderada negativa em relação à execução orçamentária e inscrição de restos a pagar na UNB; há correlação moderada positiva entre os restos a pagar e a execução financeira do orçamento na UFGD e na UNB, e correlação negativa na UFG. Apresenta-se a proposta de intervenção por meio de duas etapas: a primeira é o levantamento das informações a respeito da situação orçamentária e financeira da IFES, através de uma planilha de controle, e a segunda etapa é a aplicação da matriz GUT nos saldos orçamentários dos restos a pagar, para priorização de encerramento de tais despesas.