Otimização e validação de método para análise simultânea de dicofol, permetrina, dieldrin, endosulfan e diclorvos em ração animal, fígado e cérebro de ratos
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Data
2010-03-29.
Autores
Carvalho, Adriana Pimentel de Almeida [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Em 2005, a Agência Nacional de Vigilância Sanitária (ANVISA) através do Programa de Análise de Resíduos em Alimentos (PARA) indicou que a população brasileira está exposta aos resíduos de pesticidas. Considerando este contexto, foi proposto um projeto temático, coordenado pelo Prof. Dr. João Lauro Viana de Camargo (Faculdade de Medicina de Botucatu-UNESP), com o apoio da Fapesp. Para investigar o efeito da exposição a baixas doses de misturas de pesticidas quanto à carcinogenicidade e alteração do sistema endócrino em ratos machos de Lewis, foram escolhidos quatro pesticidas dentre os mais encontrados pela ANVISA (2005) em frutas e vegetais consumidos no país: diclorvos, dicofol, permetrina (cis-trans), dieldrin e endosulfan (α- ß). Na avaliação da toxicidade destes pesticidas e sua eventual importância para a saúde humana foram utilizados modelos com ratos machos da linhagem de Lewis expostos a esses agentes por via oral durante 8 semanas alimentados com uma ração basal enriquecida com os pesticidas nas concentrações NOEL e LOEL. Como parte do referido projeto temático, o desenvolvimento deste trabalho contempla a otimização e validação de métodos analíticos para a quantificação dos pesticidas selecionados em amostras de ração e tecidos provenientes dos animais de experimentação (fígado e cérebro). É parte fundamental deste projeto, a garantia da dose que estará sendo ingerida pelo animal, por isso foi desenvolvido e validado um método para análise dos pesticidas na ração animal. 0,5 g da amostra de ração triturada e homogeneizada foi extraída com 5 mL de acetato de etila em banho de ultrassom por 20 minutos seguido de centrifugação. O sobrenadante foi concentrado até à secura sob suave corrente de nitrogênio, redissolvido em 1,0 mL de isooctano e 1µL foi analisado por GC/ECD. Os parâmetros de validação...
In 2005, the National Health Surveillance Agency through the program for the analysis of residues in foods indicated that the Brazilian population was exposed to pesticide residues. Considering this context, a thematic project was proposed, under Prof. Dr. João Lauro Viana de Camargo (Faculdade de Medicina de Botucatu-UNESP), with FAPESP financial support. In order to investigate the carcinogenic and endocrine effect of exposure to low doses of pesticide mixtures in Lewis male mice, were chosen four types of pesticides found in fruits and vegetables by ANVISA survey in 2005. The selected pesticides were: dichlorvos, dicofol, permethrin (cis-trans), dieldrin and endosulfan (α- β). The toxicity evaluation of these pesticides was carried out in Lewis male mice fed for 8 weeks with a basal ration enriched with pesticides at concentrations NOEL and LOEL. The main purpose of this work was to optimize and validate analytical methods for determination pesticides in samples of feed and tissue from the experimental animals (liver and brain). The security of dose in animal feed was also developed and validated; 0.5 g sample of feed was triturated, homogenized and extracted with 5 mL of ethyl acetate in ultrasonic bath for 20 minutes followed by centrifugation. The supernatant was concentrated to dryness in a gentle stream of nitrogen, dissolved in 1.0 mL of isooctane and 1 µL was analyzed by GC / ECD. The validation parameters of the method were: recovery of 70 to 99 %, accuracy of less than 10 % (coefficient of variation) and quantification limits LQ between 0.4 and 0.8 mg/g. The proposed method for analysis of mice liver samples was the extraction of pesticides with ethyl acetate in ultrasonic bath followed by cleanup on florisil cartridges (500 mg). The triturated and homogenized liver sample was initially transferred to a glass tube with lid containing 5 mL of ethyl... (Complete abstract click electronic access below)
In 2005, the National Health Surveillance Agency through the program for the analysis of residues in foods indicated that the Brazilian population was exposed to pesticide residues. Considering this context, a thematic project was proposed, under Prof. Dr. João Lauro Viana de Camargo (Faculdade de Medicina de Botucatu-UNESP), with FAPESP financial support. In order to investigate the carcinogenic and endocrine effect of exposure to low doses of pesticide mixtures in Lewis male mice, were chosen four types of pesticides found in fruits and vegetables by ANVISA survey in 2005. The selected pesticides were: dichlorvos, dicofol, permethrin (cis-trans), dieldrin and endosulfan (α- β). The toxicity evaluation of these pesticides was carried out in Lewis male mice fed for 8 weeks with a basal ration enriched with pesticides at concentrations NOEL and LOEL. The main purpose of this work was to optimize and validate analytical methods for determination pesticides in samples of feed and tissue from the experimental animals (liver and brain). The security of dose in animal feed was also developed and validated; 0.5 g sample of feed was triturated, homogenized and extracted with 5 mL of ethyl acetate in ultrasonic bath for 20 minutes followed by centrifugation. The supernatant was concentrated to dryness in a gentle stream of nitrogen, dissolved in 1.0 mL of isooctane and 1 µL was analyzed by GC / ECD. The validation parameters of the method were: recovery of 70 to 99 %, accuracy of less than 10 % (coefficient of variation) and quantification limits LQ between 0.4 and 0.8 mg/g. The proposed method for analysis of mice liver samples was the extraction of pesticides with ethyl acetate in ultrasonic bath followed by cleanup on florisil cartridges (500 mg). The triturated and homogenized liver sample was initially transferred to a glass tube with lid containing 5 mL of ethyl... (Complete abstract click electronic access below)
Descrição
Palavras-chave
Quimica analitica, Pesticidas, Cromatografia gasosa, Analytical chemistry, Pesticides, Gas chromatography
Como citar
CARVALHO, Adriana Pimentel de Almeida. Otimização e validação de método para análise simultânea de dicofol, permetrina, dieldrin, endosulfan e diclorvos em ração animal, fígado e cérebro de ratos. 2010. 134 f. Tese (doutorado) - Universidade Estadual Paulista, Instituto de Química, 2010.