Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência

Detalhes bibliográficos
Autor(a) principal: Ane Patricia Cacique
Data de Publicação: 2012
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Repositório Institucional da UFMG
Texto Completo: http://hdl.handle.net/1843/NCAP-94LQ6J
Resumo: Mycotoxins are toxic substances produced by fungi that can be found in many foods, such as grapes and processed foods (grape juice, wine and raisins). Ochratoxin A (OTA) naturally occurring belongs to the group of the ochratoxins and its structure is considered to be the most toxic. The analysis of this mycotoxin is performed using liquid-liquid extraction, but this method has a high solvent consumption and needs a cleaning step of the extracts before quantitative analyzes. Studies have been conducted using immunoaffinity columns. However, this technique presents high costs. OTA detection is usually performed by high performance liquid chromatography coupled to the fluorescence detector and mass. Given this scenario, the present work aimed to optimize and validate an alternative analytical method for analysis of ochratoxin A in grapes and processed products. For this, we used two extraction techniques (liquid-liquid partition at low temperature and solid-liquid purification at low temperature) for identification and quantification of ochratoxin A in samples of grape juice, wine, raisins and pink grapes. The experiments were performed at the Research Laboratory of Agrochemistry ICA / UFMG. The influence of ionic strength, pH and the mode of homogenization in the percentages of extraction of ochratoxin A were evaluated. The analyzes were conducted by high performance liquid chromatography with ultraviolet detector (HPLC-UV). The techniques showed extraction percentages higher than 66%, and standard deviation of less than 10%. Ochratoxin A was quantified as derivatized with lower detection limits of 12.5 mg kg-1 to the solid matrices and 6.25 g L-1 for liquid matrices. The limits of quantification were 41.63 mg kg-1 and equal to 20.88 mg L-1, respectively. The chromatographic response was linear for ochratoxin A derivatized with determination coefficient higher than 0.99 in all four matrices analyzed.
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spelling Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiênciaOTA derivatizadaCLAE-UVOTACiências AgráriasMycotoxins are toxic substances produced by fungi that can be found in many foods, such as grapes and processed foods (grape juice, wine and raisins). Ochratoxin A (OTA) naturally occurring belongs to the group of the ochratoxins and its structure is considered to be the most toxic. The analysis of this mycotoxin is performed using liquid-liquid extraction, but this method has a high solvent consumption and needs a cleaning step of the extracts before quantitative analyzes. Studies have been conducted using immunoaffinity columns. However, this technique presents high costs. OTA detection is usually performed by high performance liquid chromatography coupled to the fluorescence detector and mass. Given this scenario, the present work aimed to optimize and validate an alternative analytical method for analysis of ochratoxin A in grapes and processed products. For this, we used two extraction techniques (liquid-liquid partition at low temperature and solid-liquid purification at low temperature) for identification and quantification of ochratoxin A in samples of grape juice, wine, raisins and pink grapes. The experiments were performed at the Research Laboratory of Agrochemistry ICA / UFMG. The influence of ionic strength, pH and the mode of homogenization in the percentages of extraction of ochratoxin A were evaluated. The analyzes were conducted by high performance liquid chromatography with ultraviolet detector (HPLC-UV). The techniques showed extraction percentages higher than 66%, and standard deviation of less than 10%. Ochratoxin A was quantified as derivatized with lower detection limits of 12.5 mg kg-1 to the solid matrices and 6.25 g L-1 for liquid matrices. The limits of quantification were 41.63 mg kg-1 and equal to 20.88 mg L-1, respectively. The chromatographic response was linear for ochratoxin A derivatized with determination coefficient higher than 0.99 in all four matrices analyzed.As micotoxinas são substâncias tóxicas produzidas por fungos que podem ser detectadas em diversos alimentos, como uva e produtos processados (suco de uva, vinho e uvas passa). A ocratoxina A (OTA) de ocorrência natural, pertence ao grupo das ocratoxinas e é considerada a estrutura mais tóxica. A análise dessa micotoxina é realizada utilizando a extração líquido-líquido, porém esse método apresenta elevado consumo de solvente e necessita de uma etapa de limpeza dos extratos antes das análises quantitativas. Estudos têm sido realizados com a utilização de colunas de imunoafinidade, entretanto, esta técnica apresenta custos elevados. A detecção de OTA, normalmente, é feita por cromatografia líquida de alta eficiência acoplada ao detector de fluorescência e de massas. Diante desse cenário, no presente trabalho, teve como objetivo otimizar e validar um método analítico alternativo para análise de ocratoxina A em uvas e produtos processados. Para isso, foram utilizadas duas técnicas de extração (líquido-líquido com partição em baixa temperatura e sólido-líquido com purificação em baixa temperatura) para identificação e quantificação de ocratoxina A em amostras de suco de uva, vinho, uvas passa e rosada. Os experimentos foram realizados no Laboratório de Pesquisa em Agroquímica do ICA/UFMG. Foram avaliadas a influência da força iônica, pH e do modo de homogeneização nas porcentagens de extração de ocratoxina A. As análises foram realizadas por cromatografia líquida de alta eficiência com detector de ultravioleta (CLAE-UV). As técnicas apresentaram porcentagens de extração superiores a 66%, e desvio padrão inferior a 10 %. A ocratoxina A foi quantificada na forma derivatizada com limites de detecção inferiores a 12,5 g Kg-1 para as matrizes sólidas e de 6,25 g L-1 para as matrizes líquidas. Os limites de quantificação foram de 41,63 g Kg-1 e iguais a 20,88 g L-1, respectivamente. A resposta cromatográfica foi linear para a ocratoxina A derivatizada, com coeficiente de determinação superior a 0,99 nas quatro matrizes analisadas.Universidade Federal de Minas GeraisUFMGGevany Paulino de PinhoFlaviano Oliveira SilverioAnna Christina de AlmeidaCharles Martins AguilarPaulo Henrique FidêncioAne Patricia Cacique2019-08-10T02:57:33Z2019-08-10T02:57:33Z2012-11-30info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttp://hdl.handle.net/1843/NCAP-94LQ6Jinfo:eu-repo/semantics/openAccessporreponame:Repositório Institucional da UFMGinstname:Universidade Federal de Minas Gerais (UFMG)instacron:UFMG2019-11-14T10:23:20Zoai:repositorio.ufmg.br:1843/NCAP-94LQ6JRepositório InstitucionalPUBhttps://repositorio.ufmg.br/oairepositorio@ufmg.bropendoar:2019-11-14T10:23:20Repositório Institucional da UFMG - Universidade Federal de Minas Gerais (UFMG)false
dc.title.none.fl_str_mv Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
title Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
spellingShingle Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
Ane Patricia Cacique
OTA derivatizada
CLAE-UV
OTA
Ciências Agrárias
title_short Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
title_full Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
title_fullStr Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
title_full_unstemmed Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
title_sort Determinação de ocratoxina A em uva e produtos processados por cromatografia líquida de alta eficiência
author Ane Patricia Cacique
author_facet Ane Patricia Cacique
author_role author
dc.contributor.none.fl_str_mv Gevany Paulino de Pinho
Flaviano Oliveira Silverio
Anna Christina de Almeida
Charles Martins Aguilar
Paulo Henrique Fidêncio
dc.contributor.author.fl_str_mv Ane Patricia Cacique
dc.subject.por.fl_str_mv OTA derivatizada
CLAE-UV
OTA
Ciências Agrárias
topic OTA derivatizada
CLAE-UV
OTA
Ciências Agrárias
description Mycotoxins are toxic substances produced by fungi that can be found in many foods, such as grapes and processed foods (grape juice, wine and raisins). Ochratoxin A (OTA) naturally occurring belongs to the group of the ochratoxins and its structure is considered to be the most toxic. The analysis of this mycotoxin is performed using liquid-liquid extraction, but this method has a high solvent consumption and needs a cleaning step of the extracts before quantitative analyzes. Studies have been conducted using immunoaffinity columns. However, this technique presents high costs. OTA detection is usually performed by high performance liquid chromatography coupled to the fluorescence detector and mass. Given this scenario, the present work aimed to optimize and validate an alternative analytical method for analysis of ochratoxin A in grapes and processed products. For this, we used two extraction techniques (liquid-liquid partition at low temperature and solid-liquid purification at low temperature) for identification and quantification of ochratoxin A in samples of grape juice, wine, raisins and pink grapes. The experiments were performed at the Research Laboratory of Agrochemistry ICA / UFMG. The influence of ionic strength, pH and the mode of homogenization in the percentages of extraction of ochratoxin A were evaluated. The analyzes were conducted by high performance liquid chromatography with ultraviolet detector (HPLC-UV). The techniques showed extraction percentages higher than 66%, and standard deviation of less than 10%. Ochratoxin A was quantified as derivatized with lower detection limits of 12.5 mg kg-1 to the solid matrices and 6.25 g L-1 for liquid matrices. The limits of quantification were 41.63 mg kg-1 and equal to 20.88 mg L-1, respectively. The chromatographic response was linear for ochratoxin A derivatized with determination coefficient higher than 0.99 in all four matrices analyzed.
publishDate 2012
dc.date.none.fl_str_mv 2012-11-30
2019-08-10T02:57:33Z
2019-08-10T02:57:33Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
format masterThesis
status_str publishedVersion
dc.identifier.uri.fl_str_mv http://hdl.handle.net/1843/NCAP-94LQ6J
url http://hdl.handle.net/1843/NCAP-94LQ6J
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Minas Gerais
UFMG
publisher.none.fl_str_mv Universidade Federal de Minas Gerais
UFMG
dc.source.none.fl_str_mv reponame:Repositório Institucional da UFMG
instname:Universidade Federal de Minas Gerais (UFMG)
instacron:UFMG
instname_str Universidade Federal de Minas Gerais (UFMG)
instacron_str UFMG
institution UFMG
reponame_str Repositório Institucional da UFMG
collection Repositório Institucional da UFMG
repository.name.fl_str_mv Repositório Institucional da UFMG - Universidade Federal de Minas Gerais (UFMG)
repository.mail.fl_str_mv repositorio@ufmg.br
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