Desenvolvimento e Validação de um Método Analítico para Quantificação de Atrazina do Fipronil e seus Produtos de Degradação em Amostras de Solo por Cromatografia Líquida de Alta Eficiência
DOI:
https://doi.org/10.5902/2179460X18889Keywords:
agrotóxico, CLAE e solo.Abstract
O uso de agrotóxicos na agricultura pode ser uma fonte de risco para a saúde humana e para o ambiente. Considerando que o solo é um dos principais destinos desses compostos após a aplicação, este estudo apresenta a validação de um método analítico para a quantificação dos resíduos de atrazina, fipronil e seus produtos de degradação (desulfinil, sulfeto e sulfona) em solo, empregando Cromatografia Líquida de Alta Eficiência (CLAE) com detector de arranjo de diodos (DAD). O método validado consiste na agitação por 1h do solo + metanol, centrifugação por 30 min, seguido de filtração. O método apresentou recuperações médias para o fipronil, dessulfinil, sulfeto, sulfona e atrazina entre 72 a 110% para ambos os solos, com valores de coeficiente de variação inferiores a 13%. Todas as curvas analíticas apresentaram coeficientes de determinação (R2) superiores a 0,999. Os limites de quantificação para o fipronil, dessulfinil, sulfeto e sulfona foram de 4 µg g-1 e para a atrazina de 2 µg g-1. O método validado mostrou-se adequado para ser aplicado com sucesso em amostras de solos.
Downloads
References
AGROFIT: Sistema de Agrotóxicos Fitossanitários. Brasília: Ministério da Agricultura, Pecuária e Abastecimento, 2003.
ANDREU, V.; PICÓ Y. Determination of pesticides and their degradation products in soil: Critical review and comparison of methods. Trends in Analytical Chemical, v. 23, p. 772 – 789, 2004.
ANVISA: Agência Nacional de Vigilância Sanitária. Resolução RE nº 899, de 29/05/2003
ARIAS-ESTEVEZ, M.; LOPEZ-PERIAGO, E.; MARTINEZ-CARBALLO, E.; SIMALGANDARA, J.; MEJUTO, J. C.; GARCIA-RIO, L. The mobility and degradation of pesticides in soils and the pollution of groundwater resources. Agriculture, Ecosystems and Environment, v.123, p. 247–260, 2008.
BASF: Disponível em: http://www.agro.basf.com.br/agr/ms/apbrazil/pt_BR/content/APBrazil/solutions/insecticides/insecticides_product/Regente_800_WG. Acesso em 27 mai. 2015.
BARCELÓ, D.; HENNION, M. C. Trace determination of pesticides and their degradation products en water. 3 ed. Amsterdam: Elsevier, 1997, 542 p.
BOBÉ, A.; COOPER, J. F.; COSTE, C. M.; MULLER, M. A. Behavior os fipronil em soil under sahelian plain field conditions. Pesticides Science, v. 52, p. 275-281, 1998.
CHOPRA, I.; CHAUHAM, R.; KUMARI, B.; DAHIYA, K. K. Fate of Fipronil in Cotton and Soil Under Tropical Climatic Conditions. Bulletin of Environmental Contamination and Toxicology, v. 86, p. 242–245, 2011.
HADJMOHAMMADI, M. R.; NIKOU, S. M.; KAMEL, K. Determination of Fipronil Residue in Soil and Water in the Rice Fields in North of Iran by RP-HPLC Method. Acta Chimica Slovenica, v. 53, p. 517–520, 2006.
HAYES, T. B.; ANDERSON, L. L.; BEASLEY, V. R.; SOLLA, S. R.; IGUCHI, T.; INGRAHAM, H.; et al. Demasculinization and feminization of male gonads by atrazine: Consistent effects across vertebrate classes. Journal of Steroid Biochemistry & Molecular Biology, v. 127 p. 64–73, 2011.
INMETRO: Instituto Nacional de Metrologia, Normalização e Qualidade Industrial. Orientações sobre Validação de Métodos de Ensaios Químicos, DOQ-CGCRE-008, 2010. Disponível em: http://www.inmetro.gov.br/Sidoq/Arquivos/CGCRE/DOQ/DOQ-CGCRE-8_03.pdf. Acesso em 10 de jun. de 2015.
MANDAL, K.; SINGH, B. Persistence of fipronil and its metabolites in sandy loam and clay loam soils under laboratory conditions. Chemosphere, v. 91, p1596–1603, 2013.
MAPA Ministério da Agricultura, Pecuária e Abastecimento. Disponível em: http :// extranet. agricultura.gov.br/agrofit_cons/principal_agrofit_ cons. Acesso em mar 2015.
MARTINAZZO, R.; DICK, D. P.; HIRSCHI, M. M.; LEITE, S. B.; PERELBA, M. C. R. Sorção da atrazina e de mesotriona em latossolo e estimativa de potencial de contaminação. Química Nova, v. 34, n. 8, p. 1378-1384, 2011.
MASUTTI, C. S. M.; MERMUT, A. R. Degradation of fipronil under laboratory conditions in a tropical soil from sirinhaém pernambuco, Brazil. Journal of Environmental Science and Health Part B, v. 42, p. 33–43, 2007.
MOHAPATRA, S.; AHUJA, A. K. Behaviour of fipronil in soil under different moisture levels. Indian Journal of Agricultural Sciences, v. 80 n. 7, p. 658–61, 2010.
MONTGOMERY, J. H. Agrochemicals, desk reference. 2 ed. Boca Raton, New York, Lews Publichers, 1997, 656p.
Pesticide Action Network-UK (PAN). (2000). Active ingredient Fact Sheet: Fipronil, Pesticides News London, v. 48, p. 5–30.
PERES, T. B.; PAPINI, S.; MARCHETTI, M.; NAKAGAWA, L. E.; MARCONDES, M. A.; ANDRÉA, M. M. ; LUCHINI, L. C. Métodos de extração de agrotóxicos de diversas matrizes, Arquivos do Instituto Biológico, v. 69, n. 4, p. 87-94, 2002.
RAMÍREZ, R. F.; ESQUIVEL, L. E. B.; MARTÍNEZ, F. D. B.; ACOSTA, I. L.; PÉREZ, M. D. O. Development and Validation of an Analytical Method to Determine Fipronil and its Degradation Products in Soil Samples. Bulletin of Environmental Contamination and Toxicology, v. 89, p. 744–750, 2012.
RIBANI, M.; BOTTOLI, C. B. G.; COLLINS, C. H.; JARDIM, I. C. S. F.; MELO, L. F. C. Validação em métodos cromatográficos e eletroforéticos. Química Nova, v. 27, p. 771-780, 2004.
SANTOS, H. G.; JACOMINE, P. K. T.; ANJOS, L. H. C.; OLIVEIRA, V. A.; OLIVEIRA, V. B.; COELHO, M. R.; et al. Sistema Brasileiro de Classificação de Solos. 2. ed. Rio de Janeiro: Solos, 2006. 306 p.
SAINI, S.; RANI, M.; KUMARI, B. Persistence of fipronil and its metabolites in soil under field conditions. Environmental Monitoring and Assessment, v. 186, n. 1, p. 69-75, 2014.
SPADOTTO , C. A.; GOMES, M. A. F.; LUCHINI, L. C.; ANDÉA, M. M. Monitoramento de risco ambiental de agrotóxicos: princípios e recomendações. Jaguariúna: Embrapa Meio Ambiente, 2004. 29 p. (Documento, 42).
THIER, H.P.; ZEUMER, H. Manual of pesticide residue analysis, New York: VHC, 1987, 218p.
U.S. EPA, 1996. New pesticide fact sheet. PB96-181516. EPA 737-F-96-005. U.S. EPA Office of Prevention, Pesticides and Toxic Substances.
Downloads
Published
How to Cite
Issue
Section
License
To access the DECLARATION AND TRANSFER OF COPYRIGHT AUTHOR’S DECLARATION AND COPYRIGHT LICENSE click here.
Ethical Guidelines for Journal Publication
The Ciência e Natura journal is committed to ensuring ethics in publication and quality of articles.
Conformance to standards of ethical behavior is therefore expected of all parties involved: Authors, Editors, Reviewers, and the Publisher.
In particular,
Authors: Authors should present an objective discussion of the significance of research work as well as sufficient detail and references to permit others to replicate the experiments. Fraudulent or knowingly inaccurate statements constitute unethical behavior and are unacceptable. Review Articles should also be objective, comprehensive, and accurate accounts of the state of the art. The Authors should ensure that their work is entirely original works, and if the work and/or words of others have been used, this has been appropriately acknowledged. Plagiarism in all its forms constitutes unethical publishing behavior and is unacceptable. Submitting the same manuscript to more than one journal concurrently constitutes unethical publishing behavior and is unacceptable. Authors should not submit articles describing essentially the same research to more than one journal. The corresponding Author should ensure that there is a full consensus of all Co-authors in approving the final version of the paper and its submission for publication.
Editors: Editors should evaluate manuscripts exclusively on the basis of their academic merit. An Editor must not use unpublished information in the editor's own research without the express written consent of the Author. Editors should take reasonable responsive measures when ethical complaints have been presented concerning a submitted manuscript or published paper.
Reviewers: Any manuscripts received for review must be treated as confidential documents. Privileged information or ideas obtained through peer review must be kept confidential and not used for personal advantage. Reviewers should be conducted objectively, and observations should be formulated clearly with supporting arguments, so that Authors can use them for improving the paper. Any selected Reviewer who feels unqualified to review the research reported in a manuscript or knows that its prompt review will be impossible should notify the Editor and excuse himself from the review process. Reviewers should not consider manuscripts in which they have conflicts of interest resulting from competitive, collaborative, or other relationships or connections with any of the authors, companies, or institutions connected to the papers.
