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Previous issue date: 2015-12-18 / A Benzilpenicilina (PENG) ? usada como princ?pio ativo em medicamentos veterin?rios, para aumentara produtividade pecu?ria, devido suas propriedades terap?uticas. Este antibi?tico ? indicado para controle de infec??es em animais produtores de alimentos, como bovinos e caprinos. Por?m, quando s?o de m? qualidade e utilizados indiscriminadamente, resultam em res?duos nos alimentos expostos ao consumo humano, principalmente, no leite que ? essencial para dieta das popula??es de crian?as e idosos. Assim, ? imprescind?vel que se desenvolvam novos m?todos capazes de detectar os res?duos nesse alimento, em n?veis que s?o nefastos a sa?de humana, a fim de contribuir com a seguran?a alimentar dos consumidores e colaborar com as ag?ncias reguladoras numa fiscaliza??o eficiente. Este trabalho oferece um novo m?todo, para determina??ode res?duos dos antibi?ticos. Aqui, mostramos duas etapas para controle anal?tico, na primeira ? constatado, pelas medidas das propriedades f?sico-qu?micas, a identidade e qualidade desses f?rmacos, comercialmente distribu?dos. Na segunda etapa, foi desenvolvido e validado um novo m?todo para extra??o, identifica??o e quantifica??o de PENG utilizando Cromatografia liquida ultra-r?pida acoplada a arranjo linear de fotodiodos (UFLC-DAD). Este m?todo foi aplicado em amostras de leite ultrapasterizado bovino (m?todo 1) e caprino (m?todo 2). O m?todo 1 apresentou limite de detec??o (LD) 7,246 ? 10-4?g mL-1. Limite de quantifica??o (LQ) 2,196 ? 10-3?g mL-1. O m?todo 2 apresentou LD de 8,251 ? 10-4 ?g mL-1. LQ de 2,5270 ? 10-3 ?g mL-1. Os resultados mostraram concord?ncia com o limite m?ximo de res?duos (LMR)de 4 ? 10-3 ?g mL-1em 88% para leite bovino e 85% para leite caprino. Os m?todos desenvolvidos se apresentam como uma excelente ferramenta a ser utilizada na investiga??o dos res?duos de antibi?ticos em leite. Sobretudo porque os procedimentos desenvolvidos apresentaram simplicidade, seletividade, reduzido tempo de an?lise e consumo de reagentes e solventes t?xicos, se comparados ?s metodologias j? estabelecidas. / The Benzylpenicillin (PENG) have been as the active ingredient in veterinary medicinal products, to increase productivity, due to its therapeutic properties. However, one of unfortunate quality and used indiscriminately, resulting in residues in foods exposed to human consumption, especially in milk that is essential to the diet of children and the ageing. Thus, it is indispensable to develop new methods able to detect this waste food, at levels that are toxic to human health, in order to contribute to the food security of consumers and collaborate with regulatory agencies in an efficient inspection. In this work, were developed methods for the quality control of veterinary drugs based on Benzylpenicillin (PENG) that are used in livestock production. Additionally, were validated methodologies for identifying and quantifying the antibiotic residues in milk bovine and caprine. For this, the analytical control was performed two steps. At first, the groups of samples of medicinal products I, II, III, IV and V, individually, were characterized by medium infrared spectroscopy (4000 ? 600 cm-1). Besides, 37 samples, distributed in these groups, were analyzed by spectroscopy in the ultraviolet and near infrared region (UV VIS NIR) and Ultra Fast Liquid Chromatograph coupled to linear arrangement photodiodes (UFLC-DAD). The results of the characterization indicated similarities, between PENG and reference standard samples, primarily in regions of 1818 to 1724 cm-1 of ? C=O that shows primary amides features of PENG. The method by UFLC-DAD presented R on 0.9991. LOD of 7.384 ? 10-4 ?g mL-1. LOQ of 2.049 ? 10-3 ?g mL-1. The analysis shows that 62.16% the samples presented purity ? 81.21%. The method by spectroscopy in the UV VIS NIR presented medium error ? 8 ? 12% between the reference and experimental criteria, indicating is a secure choice for rapid determination of PENG. In the second stage, was acquiring a method for the extraction and isolation of PENG by the addition of buffer McIlvaine, used for precipitation of proteins total, at pH 4.0. The results showed excellent recovery values PENG, being close to 92.05% of samples of bovine milk (method 1). While samples of milk goats (method 2) the recovery of PENG were 95.83%. The methods for UFLC-DAD have been validated in accordance with the maximum residue limit (LMR) of 4 ?g Kg-1 standardized by CAC/GL16. Validation of the method 1 indicated R by 0.9975. LOD of 7.246 ? 10-4 ?g mL-1. LOQ de 2.196 ? 10-3 ?g mL-1. The application of the method 1 showed that 12% the samples presented concentration of residues of PENG > LMR. The method 2 indicated R by 0.9995. LOD 8.251 ? 10-4 ?g mL-1. LOQ de 2.5270 ? 10-3 ?g mL-1. The application of the method showed that 15% of the samples were above the tolerable. The comparative analysis between the methods pointed better validation for LCP samples, because the reduction of the matrix effect, on this account the tcalculs < ttable, caused by the increase of recovery of the PENG. In this mode, all the operations developed to deliver simplicity, speed, selectivity, reduced analysis time and reagent use and toxic solvents, particularly if compared to the established methodologies.
| Identifer | oai:union.ndltd.org:IBICT/oai:repositorio.ufrn.br:123456789/20855 |
| Date | 18 December 2015 |
| Creators | Cabral, Alessandra Miranda |
| Contributors | 31482015404, http://lattes.cnpq.br/2959800336802498, Fernandes, Nedja Suely, 44420773472, http://lattes.cnpq.br/9563490368583906, Silva, Henrique Eduardo Bezerra da, 48102288434, http://lattes.cnpq.br/2722164837738303, Melo, Jailson Vieira de, 50073788449, http://lattes.cnpq.br/7275955550556570, Santos, Klecia Morais dos, 00836353439, http://lattes.cnpq.br/7924455214362992, Maciel, Maria In?s Sucupira, 15065766134, http://lattes.cnpq.br/2091651168946523, Silva, Djalma Ribeiro da, Moura, Maria de F?tima Vit?ria de |
| Publisher | Universidade Federal do Rio Grande do Norte, PROGRAMA DE P?S-GRADUA??O EM QU?MICA, UFRN, Brasil |
| Source Sets | IBICT Brazilian ETDs |
| Language | Portuguese |
| Detected Language | English |
| Type | info:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/doctoralThesis |
| Source | reponame:Repositório Institucional da UFRN, instname:Universidade Federal do Rio Grande do Norte, instacron:UFRN |
| Rights | info:eu-repo/semantics/openAccess |
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