Determina??o de fipronil e fipronil sulfona em ?guas superficiais da bacia do rio Guandu por Cromatografia L?quida de Alta Efici?ncia acoplada ? espectrometria de massas

• Ano de defesa: 2022
• Autor(a) principal: Ferreira, Thais Paes
• Orientador(a): Cid, Yara Peluso
• Banca de defesa: Peluso, Yara, Castro, Rosane Nora, Nascentes, Alexandre Lioi, Albert, Andr? Lu?s Mazzei, Padilha, M?nica Costa
• Tipo de documento: Tese
• Tipo de acesso: Acesso aberto
• Idioma: por
• Instituição de defesa: Universidade Federal Rural do Rio de Janeiro
• Programa de Pós-Graduação: Programa de P?s-Gradua??o em Qu?mica
• Departamento: Instituto de Qu?mica
• País: Brasil
• Palavras-chave em Português: Inseticida; Rio Guandu; ?gua Superficial; LC-MS; Contamina??o
• Palavras-chave em Inglês: Insecticide; River Guandu; Surface Water; Contamination
• Área do conhecimento CNPq: Qu?mica
• Link de acesso: https://tede.ufrrj.br/jspui/handle/jspui/5638

Fipronil (FIP) is a broad spectrum insecticide used in several sectors, which presents environmental and human health risks. In several countries, studies report the presence of FIP and its degradation products in several aquatic environments, being fipronil sulfone (FIP-S) one of the most commonly found degradation products. However, its occurrence in surface waters in Brazil is limited. Within this context, the objective of this work was to develop and validate an analytical method using solid phase extraction (SPE) and liquid chromatography coupled to mass spectrometry (LC-MS), capable of evaluating the presence of FIP and FIP-S in water from the Guandu river basin, Rio de Janeiro, Brazil. The detection limits of the method calculated for FIP and FIP-S were respectively 0.025 ?g / L and 0.014 ?g / L, while the limits of quantification of the method were 0.10 ?g / L and 0.050 ?g / L. The method presented is linear in the range of 25-300 ?g / L for FIP and 50-300 ?g / L for FIP-S, with coefficients of determination equal to 0.99. Accuracy values of 70.8-110 and precision with standard deviation relative to 20% were found under repeatability (intraday) and intermediate (interday) conditions. The proposed method was proposed for the analysis of 16 samples collected in two seasons in 2020: summer and autumn, in eight sampling points in the Guandu river basin, in the State of Rio de Janeiro. FIP was found in 75% of the evaluated samples), in the range of 0.132 - 2.44 ?g / L, while FIP-S was quantified in only one sample (0.135 ?g / L), but it was possible to detect the presence of this analyte in 62.5% of the samples. This is the first study of the occurrence of FIP and FIP-S in the Guandu river basin. The developed method is sensitive, fast and has high selectivity, allowing the identification and quantification of FIP and FIP-S in a very important region of the city of Rio de Janeiro. The results point to the concern of a possible contamination of the water supply and the need to include this pesticide and its derivatives in the surface water quality legislation.