Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil

Detalhes bibliográficos
Autor(a) principal: Oliveira, Maurício Schneider
Data de Publicação: 2010
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Biblioteca Digital de Teses e Dissertações do UFSM
Texto Completo: http://repositorio.ufsm.br/handle/1/5689
Resumo: Mycotoxins are toxic substances resulting from the secondary metabolism of different strains of fungi. Among the known mycotoxins, aflatoxins are considered the most important, due to its presence and magnitude of contamination in food intended for human consumption and animal. From the observation that milk-producing animals that consume feed contaminated with aflatoxin B1 aflatoxin M1 will excrete in their milk, it is necessary to develop mechanisms for accurate and reliable analysis of this contaminant. Milk is one of the most complete foods "naturally" available for man, with a balanced composition of nutrients; their consumption is recommended for all stages of human development, especially in the early stages of life. This work validated a methodology for analysis of aflatoxin M1 in fluid milk and milk powder, based on the extraction and purification with immunoaffinity column with subsequent separation and detection by liquid chromatography coupled to high performance tandem mass spectrometry. The limits of detection and quantification were determined 0.003 and 0.007 μg L-1 for fluid milk and 0.003 and 0.125 μg L-1 for milk powder. The coefficients of global recovery for the method of extraction of aflatoxin M1 were 95.2% for fluid milk and 95.9% for milk powder, with a standard deviation of 5.7% and 5.3% respectively. Following the development and validation of the analytical method was a study of the occurrence of aflatoxin M1 in milk samples and fluid samples of milk powder. At a total, 173 samples were analyzed, being 123 of them for fluid milk, divided into: 23 raw milk samples, 21 samples of pasteurized milk, and 79 samples of milk UHT; obtained from outlets in the three states of southern Brazil. For milk powder were analyzed 50 samples obtained from retailers in the state of Rio Grande do Sul. The results showed an incidence of positivity of 90.2% (111) in samples of fluid milk in concentration levels from 0.01 - 0.60 μg L-1 with an average contamination of 0.07 μg L-1. For samples of milk powder, 100% (50) were contaminated at levels of concentration from 0.06 - 1.58 μg L-1 with average contamination of 0.54 μg L-1. For samples of liquid milk, 46% (57) exceeded the maximum permitted levels of aflatoxin M1 in milk, proposed by the European Union legislation (0.05 μg L-1) and 0.8% (1) exceeded the proposed maximum permitted by Brazilian legislation (0.5 μg L-1). For the samples of milk powder, 98% (49) exceeded the maximum allowed by the proposed European Union legislation. Based on these results, the method was sensitive and suitable for determination of aflatoxin M1 levels proposed by the Brazilian and European legislations. The high occurrence of aflatoxin M1 in the samples suggests that the monitoring of aflatoxin M1 in milk should be a continuous process in our region.
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spelling 2010-08-112010-08-112010-03-11OLIVEIRA, Maurício Schneider. VALIDATION OF ANALYTICAL METHOD FOR ANALYSIS OF AFLATOXIN M1 AND MILK CONTAMINATION TRADED IN THE SOUTH OF BRAZIL. 2010. 107 f. Dissertação (Mestrado em Ciência e Tecnologia dos Alimentos) - Universidade Federal de Santa Maria, Santa Maria, 2010.http://repositorio.ufsm.br/handle/1/5689Mycotoxins are toxic substances resulting from the secondary metabolism of different strains of fungi. Among the known mycotoxins, aflatoxins are considered the most important, due to its presence and magnitude of contamination in food intended for human consumption and animal. From the observation that milk-producing animals that consume feed contaminated with aflatoxin B1 aflatoxin M1 will excrete in their milk, it is necessary to develop mechanisms for accurate and reliable analysis of this contaminant. Milk is one of the most complete foods "naturally" available for man, with a balanced composition of nutrients; their consumption is recommended for all stages of human development, especially in the early stages of life. This work validated a methodology for analysis of aflatoxin M1 in fluid milk and milk powder, based on the extraction and purification with immunoaffinity column with subsequent separation and detection by liquid chromatography coupled to high performance tandem mass spectrometry. The limits of detection and quantification were determined 0.003 and 0.007 μg L-1 for fluid milk and 0.003 and 0.125 μg L-1 for milk powder. The coefficients of global recovery for the method of extraction of aflatoxin M1 were 95.2% for fluid milk and 95.9% for milk powder, with a standard deviation of 5.7% and 5.3% respectively. Following the development and validation of the analytical method was a study of the occurrence of aflatoxin M1 in milk samples and fluid samples of milk powder. At a total, 173 samples were analyzed, being 123 of them for fluid milk, divided into: 23 raw milk samples, 21 samples of pasteurized milk, and 79 samples of milk UHT; obtained from outlets in the three states of southern Brazil. For milk powder were analyzed 50 samples obtained from retailers in the state of Rio Grande do Sul. The results showed an incidence of positivity of 90.2% (111) in samples of fluid milk in concentration levels from 0.01 - 0.60 μg L-1 with an average contamination of 0.07 μg L-1. For samples of milk powder, 100% (50) were contaminated at levels of concentration from 0.06 - 1.58 μg L-1 with average contamination of 0.54 μg L-1. For samples of liquid milk, 46% (57) exceeded the maximum permitted levels of aflatoxin M1 in milk, proposed by the European Union legislation (0.05 μg L-1) and 0.8% (1) exceeded the proposed maximum permitted by Brazilian legislation (0.5 μg L-1). For the samples of milk powder, 98% (49) exceeded the maximum allowed by the proposed European Union legislation. Based on these results, the method was sensitive and suitable for determination of aflatoxin M1 levels proposed by the Brazilian and European legislations. The high occurrence of aflatoxin M1 in the samples suggests that the monitoring of aflatoxin M1 in milk should be a continuous process in our region.Micotoxinas são substâncias tóxicas resultantes do metabolismo secundário de diversas linhagens de fungos. Dentre as micotoxinas conhecidas, as aflatoxinas são consideradas as de maior importância devido a sua presença e magnitude de contaminação em alimentos destinados ao consumo humano e animal. A partir da observação de que animais produtores de leite que consumam ração contaminada com aflatoxina B1 irão excretar aflatoxina M1 em seu leite, faz-se necessário o desenvolvimento de mecanismos seguros e confiáveis para análise deste contaminante. O leite é um dos mais completos alimentos disponíveis in natura para o homem, apresentando uma balanceada composição em nutrientes, sendo seu consumo recomendado em todas as etapas de desenvolvimento do ser humano, principalmente nas fases iniciais da vida. Neste trabalho foi validada uma metodologia de análise de aflatoxina M1 em leite fluido e em pó, baseada em extração e purificação com coluna de imunoafinidade com posterior separação e detecção por cromatografia líquida de alta eficiência acoplada a espectrometria de massas sequencial. Os limites de detecção e quantificação determinados foram 0,003 e 0,007 μg L-1 para leite fluido e 0,003 e 0,125 μg L-1 para leite em pó. Os coeficientes de recuperação globais para o método de extração de aflatoxina M1 foram 95,2% para leite fluido e 95,9% para leite em pó, com desvio padrão relativo de 5,7% e 5,3%, respectivamente. Em seguida ao desenvolvimento e validação do método analítico foi realizado um estudo de ocorrência de aflatoxina M1 em amostras de leite fluido e de leite em pó. No total foram analisadas 173 amostras, sendo 123 de leite fluido, divididas em: 23 amostras de leite cru, 21 amostras de leite pasteurizado e 79 amostras de leite UHT, obtidas em estabelecimentos comerciais nos três estados da região sul do Brasil e 50 amostras de leite em pó, obtidas em estabelecimentos comerciais do estado do Rio Grande do sul. Os resultados encontrados mostram uma ocorrência de positividade de 90,2% (111) nas amostras de leite fluido, em níveis de concentração de 0,01 - 0,60 μg L-1 com contaminação média de 0,07 μg L-1. Para as amostras de leite em pó, 100% (50) estavam contaminadas, em níveis de concentração de 0,06 - 1,58 μg L-1 com contaminação média de 0,54 μg L-1. Das amostras de leite fluido 46% (57) excederam os limites máximos permitidos de aflatoxina M1 em leite, propostos pela legislação da União Européia (0,05 μg L-1) e 0,8% (1) excederam os limites máximos permitidos propostos pela legislação brasileira (0,5 μg L-1). Em relação às amostras de leite em pó, 98% (49) excederam os limites máximos permitidos propostos pela legislação da União Européia. Baseado nos resultados encontrados o método mostrou-se sensível e adequado para determinação de aflatoxina M1 nos níveis propostos pelas legislações brasileira e européia. A alta ocorrência de aflatoxina M1 nas amostras analisadas sugere que o monitoramento da aflatoxina M1 em leite deve ser um procedimento contínuo em nossa região.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em Ciência e Tecnologia dos AlimentosUFSMBRCiência e Tecnologia dos AlimentosAflatoxina M1LeiteValidaçãoAflatoxin M1MilkValidationCNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOSValidação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do BrasilValidation of analytical method for analysis of aflatoxin M1 and milk contamination traded in the south of Brazilinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisKubota, Ernesto Hashimehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788191J1Mallmann, Carlos Augustohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4782275D6Batatinha, Maria José Moreirahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4766383P7http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4508040T9Oliveira, Maurício Schneider5007000000064005005003003005ebbf8d4-22d6-44d2-914f-49fd8823c51499d19df4-2d59-4756-9b53-41ab1ae8c6bb0e52e3ae-0907-49fe-98ad-b698da7f29437c067ce9-cc65-4ac2-8f97-c2e702f9d00finfo:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALOLIVEIRA, MAURICIO SCHNEIDER.pdfapplication/pdf2276015http://repositorio.ufsm.br/bitstream/1/5689/1/OLIVEIRA%2c%20MAURICIO%20SCHNEIDER.pdf6d82d5964ad604fd494873eb7e016b50MD51TEXTOLIVEIRA, MAURICIO SCHNEIDER.pdf.txtOLIVEIRA, MAURICIO SCHNEIDER.pdf.txtExtracted texttext/plain200429http://repositorio.ufsm.br/bitstream/1/5689/2/OLIVEIRA%2c%20MAURICIO%20SCHNEIDER.pdf.txt14b6aed932eabd4ceffe706a7aad7612MD52THUMBNAILOLIVEIRA, MAURICIO SCHNEIDER.pdf.jpgOLIVEIRA, MAURICIO SCHNEIDER.pdf.jpgIM Thumbnailimage/jpeg5289http://repositorio.ufsm.br/bitstream/1/5689/3/OLIVEIRA%2c%20MAURICIO%20SCHNEIDER.pdf.jpgc9aeefcc14046848a5aad7a52b8cd888MD531/56892021-10-05 15:29:18.31oai:repositorio.ufsm.br:1/5689Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2021-10-05T18:29:18Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
dc.title.alternative.eng.fl_str_mv Validation of analytical method for analysis of aflatoxin M1 and milk contamination traded in the south of Brazil
title Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
spellingShingle Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
Oliveira, Maurício Schneider
Aflatoxina M1
Leite
Validação
Aflatoxin M1
Milk
Validation
CNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS
title_short Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
title_full Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
title_fullStr Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
title_full_unstemmed Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
title_sort Validação de metodologia analítica para análise de aflatoxina M1 e sua ocorrência no leite bovino comercializado no sul do Brasil
author Oliveira, Maurício Schneider
author_facet Oliveira, Maurício Schneider
author_role author
dc.contributor.advisor1.fl_str_mv Kubota, Ernesto Hashime
dc.contributor.advisor1Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788191J1
dc.contributor.referee1.fl_str_mv Mallmann, Carlos Augusto
dc.contributor.referee1Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4782275D6
dc.contributor.referee2.fl_str_mv Batatinha, Maria José Moreira
dc.contributor.referee2Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4766383P7
dc.contributor.authorLattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4508040T9
dc.contributor.author.fl_str_mv Oliveira, Maurício Schneider
contributor_str_mv Kubota, Ernesto Hashime
Mallmann, Carlos Augusto
Batatinha, Maria José Moreira
dc.subject.por.fl_str_mv Aflatoxina M1
Leite
Validação
topic Aflatoxina M1
Leite
Validação
Aflatoxin M1
Milk
Validation
CNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS
dc.subject.eng.fl_str_mv Aflatoxin M1
Milk
Validation
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS
description Mycotoxins are toxic substances resulting from the secondary metabolism of different strains of fungi. Among the known mycotoxins, aflatoxins are considered the most important, due to its presence and magnitude of contamination in food intended for human consumption and animal. From the observation that milk-producing animals that consume feed contaminated with aflatoxin B1 aflatoxin M1 will excrete in their milk, it is necessary to develop mechanisms for accurate and reliable analysis of this contaminant. Milk is one of the most complete foods "naturally" available for man, with a balanced composition of nutrients; their consumption is recommended for all stages of human development, especially in the early stages of life. This work validated a methodology for analysis of aflatoxin M1 in fluid milk and milk powder, based on the extraction and purification with immunoaffinity column with subsequent separation and detection by liquid chromatography coupled to high performance tandem mass spectrometry. The limits of detection and quantification were determined 0.003 and 0.007 μg L-1 for fluid milk and 0.003 and 0.125 μg L-1 for milk powder. The coefficients of global recovery for the method of extraction of aflatoxin M1 were 95.2% for fluid milk and 95.9% for milk powder, with a standard deviation of 5.7% and 5.3% respectively. Following the development and validation of the analytical method was a study of the occurrence of aflatoxin M1 in milk samples and fluid samples of milk powder. At a total, 173 samples were analyzed, being 123 of them for fluid milk, divided into: 23 raw milk samples, 21 samples of pasteurized milk, and 79 samples of milk UHT; obtained from outlets in the three states of southern Brazil. For milk powder were analyzed 50 samples obtained from retailers in the state of Rio Grande do Sul. The results showed an incidence of positivity of 90.2% (111) in samples of fluid milk in concentration levels from 0.01 - 0.60 μg L-1 with an average contamination of 0.07 μg L-1. For samples of milk powder, 100% (50) were contaminated at levels of concentration from 0.06 - 1.58 μg L-1 with average contamination of 0.54 μg L-1. For samples of liquid milk, 46% (57) exceeded the maximum permitted levels of aflatoxin M1 in milk, proposed by the European Union legislation (0.05 μg L-1) and 0.8% (1) exceeded the proposed maximum permitted by Brazilian legislation (0.5 μg L-1). For the samples of milk powder, 98% (49) exceeded the maximum allowed by the proposed European Union legislation. Based on these results, the method was sensitive and suitable for determination of aflatoxin M1 levels proposed by the Brazilian and European legislations. The high occurrence of aflatoxin M1 in the samples suggests that the monitoring of aflatoxin M1 in milk should be a continuous process in our region.
publishDate 2010
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dc.identifier.citation.fl_str_mv OLIVEIRA, Maurício Schneider. VALIDATION OF ANALYTICAL METHOD FOR ANALYSIS OF AFLATOXIN M1 AND MILK CONTAMINATION TRADED IN THE SOUTH OF BRAZIL. 2010. 107 f. Dissertação (Mestrado em Ciência e Tecnologia dos Alimentos) - Universidade Federal de Santa Maria, Santa Maria, 2010.
dc.identifier.uri.fl_str_mv http://repositorio.ufsm.br/handle/1/5689
identifier_str_mv OLIVEIRA, Maurício Schneider. VALIDATION OF ANALYTICAL METHOD FOR ANALYSIS OF AFLATOXIN M1 AND MILK CONTAMINATION TRADED IN THE SOUTH OF BRAZIL. 2010. 107 f. Dissertação (Mestrado em Ciência e Tecnologia dos Alimentos) - Universidade Federal de Santa Maria, Santa Maria, 2010.
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