Aspectos analíticos e regulatórios na determinação de resíduos de macrolídeos em alimentos de origem animal por cromatografia líquida associada à espectrometria de massas

This is an overview of LC-MS techniques applied for macrolide determination in food, including sample preparation and method validation, as well as the policies adopted by international agencies regarding their presence in food. Techniques for the analysis of macrolides in food normally include solid phase or liquid-liquid extraction followed by HPLC. UHPLC presents advantages in running time, detectability and solvent consumption. Triple-quadrupoles are the most common analyzers in instruments used for the determination of contaminants in food, but time-of-flight and ion-trap spectrometers have been successfully applied for analyses focusing on the investigation of structural formula or the presence of degradation products

Analytical and regulatory aspects for determination of macrolide residues in animal-derived foods by liquid chromatography associated with mass spectrometry

This is an overview of LC-MS techniques applied for macrolide determination in food, including sample preparation and method validation, as well as the policies adopted by international agencies regarding their presence in food. Techniques for the analysis of macrolides in food normally include solid phase or liquid-liquid extraction followed by HPLC. UHPLC presents advantages in running time, detectability and solvent consumption. Triple-quadrupoles are the most common analyzers in instruments used for the determination of contaminants in food, but time-of-flight and ion-trap spectrometers have been successfully applied for analyses focusing on the investigation of structural formula or the presence of degradation products.44946

Development and validation of analytical method using LC-MS/MS for the determination of macrolides in Nile tilapia (Oreochomis niloticus) meat

Orientador: Felix Guillermo Reyes ReyesDissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de AlimentosResumo: O resumo poserá ser visualizado no texto completo da tese digitalAbstract: The abstract is available with the full eletronic digital documentMestradoMestre em Ciência de Alimento

The rate structure of electric power distribution networks in Brazil: critical analysis of the current model and new methodological proposal.

O trabalho discute a questão da precificação eficiente em sistemas de distribuição de energia, abordando desde a teoria econômica clássica aplicada aos modelos de produção e transporte da energia, passando por uma avaliação crítica da atual metodologia de estrutura tarifária vigente no Brasil, até o detalhamento de uma proposta consistente e simplificadora de estrutura de preços para a atividade da distribuição de energia. A teoria de monopólios naturais é o pano de fundo para uma discussão integrada dos modelos clássicos de estrutura de preços para o transporte da energia elétrica. Nesta avaliação do estado da arte, são abordadas as teorias da precificação linear, da precificação não linear e da precificação de ponta. A atual metodologia nacional de cálculo da estrutura tarifária de uso das redes de distribuição, aplicada pela Agência Nacional de Energia Elétrica ANEEL, é revisitada sob uma visão técnica crítica. Como resultado, são desconstruídos alguns conceitos e processos vigentes pela constatação de uma excessiva complexidade operacional aliada a uma carência de fundamentação econômica e matemática. Por fim, é proposta uma metodologia simplificadora para a estrutura de preços de uso das redes de distribuição de energia, objetivando maior eficiência econômica, maior simplicidade operacional na aplicação e sólida fundamentação teórica, reduzindo arbitrariedades e subjetividades existentes na atual metodologia.The present work discusses the question of efficient pricing on electric power distribution systems. The subject is approached from the discussion of the classical economic theory applied to energy production and transport models, passing through a critical evaluation of the current rate structure used in Brazil, to the description of a consistent and simplified proposal for the electric power distribution rate design. The theory of natural monopolies is the background of an integrated discussion on classical rate design models concerning the electric energy transportation activity. By the classical problem analysis, some theories commonly approached are linear pricing, non linear pricing and peak load pricing. The current Brazilian methodology used for the rate design of the usage of distribution networks, applied by the National Regulatory Agency (ANEEL), is revisited under a critical technical vision. As a result, some concepts are reassessed due to the observed excessive operational complexity allied to the lack of economical and statistical foundation. Finally, a simplified methodology for the rate structure of the usage of electrical distribution networks is proposed. The methodology aims, at the same time, greater economic efficiency, simpler operational application and a solid theoretical foundation, thereby reducing arbitrariness and subjectivity found in the current methodology

Analytical And Regulatory Aspects For Determination Of Macrolide Residues In Animal-derived Foods By Liquid Chromatography Associated With Mass Spectrometry [aspectos AnalÍticos E RegulatÓrios Na DeterminaÇ Ão De ResÍduos De MacrolÍdeos Em Alimentos De Origem Animal Por Cromatografia LÍquida Associada À Espectrometria De Massas]

This is an overview of LC-MS techniques applied for macrolide determination in food, including sample preparation and method validation, as well as the policies adopted by international agencies regarding their presence in food. Techniques for the analysis of macrolides in food normally include solid phase or liquid-liquid extraction followed by HPLC. UHPLC presents advantages in running time, detectability and solvent consumption. Triple-quadrupoles are the most common analyzers in instruments used for the determination of contaminants in food, but time-of-flight and ion-trap spectrometers have been successfully applied for analyses focusing on the investigation of structural formula or the presence of degradation products.363449461Horie, M., (1995) Chemical Analysis for Antibiotics Used in Agriculture, , Oka, H.Nakazawa, H.Harada, K.MacNeil, J. D., eds.AOAC International: Arlington, chap. 6Gustafson, R.H., Bowen, R.E., (1997) J. Appl. 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A Simple Liquid Chromatography Coupled To Quadrupole Time Of Flight Mass Spectrometry Method For Macrolide Determination In Tilapia Fillets

A method for the identification and quantification of macrolides (erythromycin, josamycin, tilmicosin, tylosin, spiramycin and neospiramycin) in tilapia fillets by liquid chromatography coupled to quadrupole time of flight mass (LC-QToF) spectrometry is presented. Sample preparation was quite simple and low cost: proteins were precipitated and the analytes were extracted with ethanol, extract was defatted with hexane and concentrated by solvent evaporation. The matrix effect was statistically demonstrated during method validation, in which matrix-matched calibration was applied. Matrix effect mechanism was clarified thanks to the capability of QToF mass spectrometer of generating full scan spectra with accurate mass measurement. The limits of quantification were at least 45% lower than the maximum residue limits. The method was able to identify the studied macrolides with relative m/z errors lower than 2.5. ppm and to monitor two fragment ions per analyte, which is in accordance with the European Community recommendations for the analysis of contaminants in foods. 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Title 21: Food and Drugs, Part 556: Tolerances for residues of new animal drugs in food, pp. 370-386. , http://www.gpoaccess.gov/cfr/index.html, USDA, Washington, DC, Retrieved from:(20.06.2011), USDA, United States Department of Agriculture(2011) Aquaculture Approved Drugs, , http://www.fda.gov/AnimalVeterinary/DevelopmentApprovalProcess/Aquaculture/ucm132954.htm, USFDA, Washington, DC, Retrieved from:(20.06.11)Wang, J., Leung, D., Analysis of macrolide antibiotic residues in eggs, raw milk, and honey using both ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry and high-performance liquid chromatography/tandem mass spectrometry (2007) Rapid Communication Mass Spectrometry, 21, pp. 3213-3222Wang, J., Analysis of macrolide antibiotics using liquid chromatography-mass spectrometry in food, biological and environmental matrices (2009) Mass Spectrometry Reviews, 28, pp. 50-9

Aglutininas anti-leptospiras em doadores de sangue

Serum samples from 450 donated blood at the Hemocenter of the Clinical Hospital in the UNESP School of Medicine at Botucatu, SP, Brazil – were submitted to Microscopic Serumagglutination (SAM) exam for leptospirosis, and presented only six reactive samples (1.33%), presenting titer 100, with two reacting with the serovar Icterohaemorrhagiae (33.3%) and four with the serovar Panama (66.7%). Analysis of the epidemiological questionnaire applied to donors revealed the following findings: 54.6% of donors had maintained contact with animals, whether at work or with their pets, principally dogs and cats; 51.8% reported the presence of rats in their residence at some moment; 51.8% did not have the habit of boiling or filtering water prior to consumption; 39.2% had frequented ponds, streams and / or waterfalls; 18.2% did not rely on a sewer and water network, or on trash collection in their neighborhood; 8.4% did not habitually wash their hands after handling animals; 5.6% resided in locations subject to frequent flooding and 4.2% did not habitually wash their food before consuming it. Despite the low seroprevalence, an association of epidemiological factors was verified that shows the need for health education activities related principally to the environment including risk factors for transmission of leptospirosis to humans.Muestras de suero de 450 donantes de sangre del Hemocentro del “Hospital das Clínicas” de la “Faculdade de Medicina de Botucatu – UNESP” fueron sometidas a la prueba de Aglutinación Microscópica para leptospirosis, habiendóse encontrado sólo seis muestras reactivas (1,33%), presentando título 100, siendo dos para el serovar Icterohaemorrhagiae (33,3%) y cuatro para el Panamá (66,7%). El análisis del cuestionario epidemiológico aplicado a los donantes reveló las siguientes informaciones: 54,6% de los donantes mantenía contacto con animales, sea en la actividad laboral o con sus mascotas, principalmente perros y gatos; 51,8% relataron la presencia de ratones en el domicilio en algún momento; 51,8% no tenían el hábito de hervir o filtrar el agua antes del consumo; 39,2% frecuentaban lagunas, riachuelos y/o cascadas; 18,2% no contaban con red de agua y albañal, ni colecta de basura en el barrio; 8,4% no tenían el hábito de lavar las manos después de manosear animales; 5,6% vivían en lugares donde ocurrían frecuentemente inundaciones y 4,2% no tenían la costumbre de lavar los alimentos antes de consumirlos. Aunque presentando baja seroprevalencia, se verifica la importancia de la asociación de factores epidemiológicos que muestran la necesidad de actividades de educación en salud relacionados principalmente a los factores ambientales como factores de riesgo para la transmisíon de la leptospirosis al hombre.Amostras de soro de 450 doadores de sangue do Hemocentro do Hospital das Clínicas da Faculdade de Medicina de Botucatu – UNESP foram submetidas à prova de Soroaglutinação Microscópica (SAM) para leptospirose, tendo-se encontrado apenas seis amostras reagentes (1,33%), apresentando título 100, sendo duas para o sorovar Icterohaemorrhagiae (33,3%) e quatro para o Panamá (66,7%). A análise do questionário epidemiológico aplicado aos doadores revelou que: 54,6% dos doadores mantinham contato com animais, seja na atividade laboral ou com seus animais de estimação, principalmente cães e gatos; 51,8% relataram a presença de ratos no domicílio em algum momento; 51,8% não tinham o hábito de ferver ou filtrar a água antes do consumo; 39,2% frequentavam lagoas, riachos e/ou cachoeiras; 18,2% não contavam com rede de água e esgoto, nem coleta de lixo no bairro; 8,4% não tinham o hábito de lavar as mãos após manusear animais; 5,6% residiam em locais onde ocorriam frequentemente enchentes e 4,2% não tinham o costume de lavar os alimentos antes de consumi-los. Apesar da baixa soroprevalência, verifica-se a importância da associação de fatores epidemiológicos que mostram a necessidade de atividades de educação em saúde relacionadas principalmente aos fatores do meio ambiente como fatores de risco para a transmissão da leptospirose ao homem.Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Parâmetros bioquímicos de felídeos selvagens (Panthera leo e Panthera tigris altaica) mantidos em cativeiro

A maioria das populações de felinos selvagens é considerada ameaçada ou em extinção devido à caça indiscriminada e à redução de seu habitat natural causada pelo homem. Devido ao número limitado de animais, essas espécies são vulneráveis às doenças e endogamia, além das alterações metabólicas e comportamentais relacionadas à mudança das condições naturais, habitat e alimentação e, ainda, à condição de cativeiro. Há poucos relatos na literatura sobre a bioquímica sérica em leões e tigres. Este estudo apresenta os parâmetros bioquímicos de 23 leões de cativeiro (Panthera leo) e 10 tigres siberianos de cativeiro (Panthera tigris altaica) do Fundação Parque Zoológico de São Paulo. Ureia; creatinina; AST; ALT; ALP; GGT; bilirrubinas totais, diretos e indiretos; proteína total; albumina; CK; lactato desidrogenase; os níveis de triglicérides, de colesterol e de glicose séricas foram determinados; e também os eletrólitos cálcio, fósforo, cloro, sódio e potássio. Não foram encontradas diferenças de parâmetros bioquímicos relacionados ao sexo de Panthera leo, mas para Panthera tigris altaica foram observados valores mais elevados de albumina em machos. Os valores obtidos neste estudo podem ser usados como referência para os indivíduos em cativeiro de Panthera leo e Panthera tigris altaica.Most populations of wild felines are now considered endangered or near extinction due to the indiscriminate hunting and the reduction of their natural habitat, caused by man. Due to the limited number of animals within a population, these species are especially vulnerable to the impacts of diseases and endogamy. In addition, wild felines are also susceptible to metabolic and behavioral changes related to a change in their natural conditions, habitat, and feeding, when the animal enters into captivity. There are few descriptions in the literature of the serum biochemistries of lions and tigers. This study presents the biochemical parameters of 23 captive lions (Panthera leo) and 10 captive Siberian tigers (Panthera tigris altaica) from the Zoological Park of the Sao Paulo Foundation. Serum urea, creatinine, total protein, albumin, total, direct and indirect bilirubin were measured. In addition, serum levels of ALT, AST, ALP, GGT, glucose, CK, lactate dehydrogenase, cholesterol, and triglycerides were determined, as well as calcium, phosphorus, chlorine, sodium, and potassium. Biochemical parameters did not differ significantly among males and females lions, but higher albumin values were observed in male Panthera tigris altaica in comparison to females. The values obtained in this study may be used as reference for captive individuals of Panthera leo and Panthera tigris altaica