Determinação de glifosato e AMPA nas águas superficiais da Bacia do Paraná 3
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Data
2018-02-20
Autores
Mendonça, Cintia Franco Rodrigues
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Atualmente, o glifosato é o herbicida de maior uso para o controle de ervas daninhas, sendo muito utilizado em culturas resistentes, como soja e milho. O glifosato é aplicado diretamente sobre a folhagem das plantas, porém uma parte acaba indo para o solo. Do solo, tanto o glifosato quanto seu metabólito, ácido aminometilfosfônico (AMPA) podem ser lixiviados para águas superficiais ou subterrâneas. Por conta disto, têm se gerado preocupações quanto ao seu potencial tóxico. A presente dissertação teve como objetivo avaliar a contaminação com glifosato e AMPA das águas superficiais de microbacias situadas na Bacia do Paraná 3 (Paraná-BR). Selecionou-se microbacias situadas próximas a regiões com plantios de soja e milho, assim como o período de coleta das amostras foi escolhido dentro do época de plantio destas culturas. Estudou-se dois métodos de preparo das amostras de água: reação de derivatização com cloroformiato de 9- fluorenilmetila (FMOC-Cl) seguida de extração e pré-concentração dos analitos com extração em fase sólida (SPE) utilizando cartuchos C18; pré-concentração dos analitos por liofilização seguida de reação de derivatização com FMOC-Cl. Para a determinação de glifosato e AMPA empregou-se cromatografia líquida de alta eficiência (HPLC) com detector de fluorescência. Os resultados demonstraram que a liofilização apresenta maior eficiência no preparo das amostras. Após a escolha do método de preparo realizou-se sua avaliação de desempenho pelos parâmetros de repetitividade, seletividade, linearidade, limite de detecção de quantificação, sensibilidade e estabilidade. Os resultados demonstraram concentrações na faixa de 0,31 a 8,13, μg L-1 de glifosato, estando abaixo da concentração máxima permitida pelas resoluções brasileiras: 65 μg L-1 para águas doces classe II (CONAMA 357/05) e 500 μg L-1 para águas de consumo (MS 2914/11); com exceção de uma amostra coletada em período chuvoso, apresentando glifosato na concentração de 65 μg L-1. O metabólito AMPA foi encontrado na faixa de 0,32 –14,78 μg L-1, estando abaixo da concentração máxima permitida pela resolução MS 2914/11: 500 μg L-1.
Today , glyphosate is the herbicide of greatest consumption for the control o f weeds, widely used in resistant crops such as soybean and corn . Glyphosate is applied directly to the foliage of plants, but part of it ends up going to the soil. From the soil, both glyphosate and its metabolite , aminomethylphosphonic acid ( AMPA ) can be carried to surface water or under ground water. Because of this, concerns have been raised about its toxic potential. In this dissertation, the objective is to evaluate the contamination of surface waters of watersheds located in the Paraná Basin 3 (Paraná - BR) with glyphosate and AMPA. Microbasin located near regions with soybean and corn plantations were chosen, as well as the period of sampling was chosen within the time of planting of these crops . Two methods of preparation of the water samples were stud ied: 9 - Fluorenylmethyl chloroformate ( FMOC - Cl ) derivatization reaction and extraction and pre - concentration of analytes with s olid p hase e xtraction (SPE) using C 18 cartridges; pre - concentration of the analytes with lyophilization followed by derivatization reaction with FMOC - Cl. High p erformance l iquid c hromatography (HPLC) with fluorescence detector was used f or glyphosate and AMPA analysis . The results showed that lyophilization has a better performance in the preparation of the samples. After the choice of the preparation method, its performance evaluation was performed based on evaluation of repeatability, selectivity, linearity, sensitivity and stability were evaluated. The results showed concentrations in the range of 0.31 to 8.13, μg L - 1 of glyphosate , being below the maximum concentration allowed by the Brazilian resolutions: 65 μg L - 1 for Class II (CONAMA 357/05) and 500 μg L - 1 for drinking water (MS 2914/11); with the exception of a sample collected in the rainy season, presenting glyphosate at the concentration of 65 μg L - 1 . The AMPA metabolite was found in the range of 0.32 - 14.78 μg L - 1 , being below the maximum concentration allowed by resolution MS 2914/11: 500 μg L - 1 .
Today , glyphosate is the herbicide of greatest consumption for the control o f weeds, widely used in resistant crops such as soybean and corn . Glyphosate is applied directly to the foliage of plants, but part of it ends up going to the soil. From the soil, both glyphosate and its metabolite , aminomethylphosphonic acid ( AMPA ) can be carried to surface water or under ground water. Because of this, concerns have been raised about its toxic potential. In this dissertation, the objective is to evaluate the contamination of surface waters of watersheds located in the Paraná Basin 3 (Paraná - BR) with glyphosate and AMPA. Microbasin located near regions with soybean and corn plantations were chosen, as well as the period of sampling was chosen within the time of planting of these crops . Two methods of preparation of the water samples were stud ied: 9 - Fluorenylmethyl chloroformate ( FMOC - Cl ) derivatization reaction and extraction and pre - concentration of analytes with s olid p hase e xtraction (SPE) using C 18 cartridges; pre - concentration of the analytes with lyophilization followed by derivatization reaction with FMOC - Cl. High p erformance l iquid c hromatography (HPLC) with fluorescence detector was used f or glyphosate and AMPA analysis . The results showed that lyophilization has a better performance in the preparation of the samples. After the choice of the preparation method, its performance evaluation was performed based on evaluation of repeatability, selectivity, linearity, sensitivity and stability were evaluated. The results showed concentrations in the range of 0.31 to 8.13, μg L - 1 of glyphosate , being below the maximum concentration allowed by the Brazilian resolutions: 65 μg L - 1 for Class II (CONAMA 357/05) and 500 μg L - 1 for drinking water (MS 2914/11); with the exception of a sample collected in the rainy season, presenting glyphosate at the concentration of 65 μg L - 1 . The AMPA metabolite was found in the range of 0.32 - 14.78 μg L - 1 , being below the maximum concentration allowed by resolution MS 2914/11: 500 μg L - 1 .
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Palavras-chave
AMPA, Bacia do Paraná 3, Liofilização, Glifosato