Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras
| Ano de defesa: | 2024 |
|---|---|
| Autor(a) principal: | |
| Orientador(a): | |
| Banca de defesa: | |
| Tipo de documento: | Dissertação |
| Tipo de acesso: | Acesso aberto |
| dARK ID: | ark:/26339/001300001bqx6 |
| Idioma: | por |
| Instituição de defesa: |
Universidade Federal de Santa Maria
Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
| Programa de Pós-Graduação: |
Não Informado pela instituição
|
| Departamento: |
Não Informado pela instituição
|
| País: |
Não Informado pela instituição
|
| Palavras-chave em Português: | |
| Link de acesso: | http://repositorio.ufsm.br/handle/1/34220 |
Resumo: | Water is the foundation of life, playing an essential role in different contexts, which makes it crucial to ensure its availability in adequate quantity and quality. To maintain water potability standards is a challenge because contemporary agriculture use pesticides to meet the global demand for food. However, this practice brings substantial risks to the environment and human health. In Brazil, drinking water potability is regulated by Ordinance GM/MS Nº 888/2021, which establishes the maximum allowable concentrations (MAC) for pesticides and their metabolites. Monitoring of pesticide residues in supply systems is carried out by the National Water Quality Surveillance Program for Human Consumption (VIGIAGUA) and the data is accessible at the Water Quality Surveillance Information System for Human Consumption (SISAGUA). Therefore, the present study aimed to: 1) Evaluate the SISAGUA database related to pesticide residues in water samples from the states of Rio Grande do Sul and São Paulo from 2014 to 2022; 2) To develop and to validate an integrated SPE-LC-MS/MS method for pesticides determination in drinking water. The evaluation of the SISAGUA database revealed that 20 out of the 27 pesticides monitored in the Brazilian water supply systems have results above the MAC, including pesticides banned for agricultural use in Brazil. Aldrin and dieldrin was the most frequently detected pesticide and were found in 40 samples, covering 52% of municipalities, in concentrations between 0.04 and 15 μg L-1. For the extraction of pesticides, the use of C18 and Oasis® HLB cartridges were evaluated, followed by elution by dichloromethane and methanol or ethyl acetate. The best results were achieved using the Oasis® HLB sorbent. The validation study showed that the calculated r2 values were ≥ 0.99 for all analytes, when the analytical curves were prepared in matrix extract, demonstrating satisfactory linearity. The spiking experiments were performed by different analysts, with a 21 days-interval demonstrated accuracy and precision at the spike concentrations of 0.2; 0.5; 1 and 3 μg L-1 (n=7), presenting average recovery percentages of 79 to 135% and relative standard deviations of repeatability (RSDr) of up to 20%. Within-laboratory reproducibility (RSDwR) showed a repeatability < 20% for all analytes at the highest spike concentration. The multiresidue method was validated for the determination of 29 pesticides. The limit of quantification was 0.2 μg L-1 and 0.5 μg L-1 for 10.3% and 89.7% of those studied pesticides, respectively. The developed method is considered suitable for determining pesticides in drinking water and can be adopted as an alternative by laboratories that receive samples collected by VIGIAGUA teams. |
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Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileirasData analysis of SISAGUA and validation method for pesticides determination in drinking water in order to comply with brazilian legislationMonitoramentoMultirresíduoSPELC-MS/MSMonitoringMultiresidueCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAWater is the foundation of life, playing an essential role in different contexts, which makes it crucial to ensure its availability in adequate quantity and quality. To maintain water potability standards is a challenge because contemporary agriculture use pesticides to meet the global demand for food. However, this practice brings substantial risks to the environment and human health. In Brazil, drinking water potability is regulated by Ordinance GM/MS Nº 888/2021, which establishes the maximum allowable concentrations (MAC) for pesticides and their metabolites. Monitoring of pesticide residues in supply systems is carried out by the National Water Quality Surveillance Program for Human Consumption (VIGIAGUA) and the data is accessible at the Water Quality Surveillance Information System for Human Consumption (SISAGUA). Therefore, the present study aimed to: 1) Evaluate the SISAGUA database related to pesticide residues in water samples from the states of Rio Grande do Sul and São Paulo from 2014 to 2022; 2) To develop and to validate an integrated SPE-LC-MS/MS method for pesticides determination in drinking water. The evaluation of the SISAGUA database revealed that 20 out of the 27 pesticides monitored in the Brazilian water supply systems have results above the MAC, including pesticides banned for agricultural use in Brazil. Aldrin and dieldrin was the most frequently detected pesticide and were found in 40 samples, covering 52% of municipalities, in concentrations between 0.04 and 15 μg L-1. For the extraction of pesticides, the use of C18 and Oasis® HLB cartridges were evaluated, followed by elution by dichloromethane and methanol or ethyl acetate. The best results were achieved using the Oasis® HLB sorbent. The validation study showed that the calculated r2 values were ≥ 0.99 for all analytes, when the analytical curves were prepared in matrix extract, demonstrating satisfactory linearity. The spiking experiments were performed by different analysts, with a 21 days-interval demonstrated accuracy and precision at the spike concentrations of 0.2; 0.5; 1 and 3 μg L-1 (n=7), presenting average recovery percentages of 79 to 135% and relative standard deviations of repeatability (RSDr) of up to 20%. Within-laboratory reproducibility (RSDwR) showed a repeatability < 20% for all analytes at the highest spike concentration. The multiresidue method was validated for the determination of 29 pesticides. The limit of quantification was 0.2 μg L-1 and 0.5 μg L-1 for 10.3% and 89.7% of those studied pesticides, respectively. The developed method is considered suitable for determining pesticides in drinking water and can be adopted as an alternative by laboratories that receive samples collected by VIGIAGUA teams.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqA água é a base da vida, desempenhando um papel essencial em diferentes contextos, o que torna crucial garantir sua disponibilidade em quantidade e qualidade adequadas. Manter os padrões de potabilidade da água é um desafio porque a agricultura contemporânea recorre ao uso de agrotóxicos para atender à demanda global por alimentos. No entanto, essa prática traz riscos substanciais para o meio ambiente e à saúde humana. No Brasil, o padrão de potabilidade da água para consumo humano é regulado pela Portaria GM/MS Nº 888/2021, que estabelece os valores máximos permitidos (VMP) para agrotóxicos e seus metabólitos. O monitoramento nos sistemas de abastecimento é realizado pelo Programa Nacional de Vigilância da Qualidade da Água para Consumo Humano (VIGIAGUA) e os dados acessíveis no Sistema de Informação de Vigilância da Qualidade da Água para Consumo Humano (SISAGUA). Sendo assim, o presente estudo teve como objetivos: 1) Avaliar o banco de dados do SISAGUA relacionado aos resíduos de agrotóxicos em amostras de água dos estados do Rio Grande do Sul e São Paulo no período de 2014 a 2022; 2) Desenvolver e validar um método integrado SPE-LC-MS/MS para determinação de agrotóxicos em água potável. A análise do banco de dados do SISAGUA revelou que 20 dos 27 agrotóxicos monitorados nos sistemas de abastecimento de água no Brasil, possuem resultados acima do VMP, incluindo agrotóxicos proibidos no país para uso agrícola. Aldrin e dieldrin foram os agrotóxicos mais frequentemente detectados e foram encontrados em 40 amostras, abrangendo 52% dos municípios, em concentrações entre 0,04 e 15 μg L-1. Para extração dos agrotóxicos avaliou-se o uso de cartuchos C18 e Oasis® HLB, seguido de eluição com diclorometano e metanol ou acetato de etila. Os melhores resultados foram alcançados utilizando o sorvente Oasis® HLB. O estudo de validação mostrou que os valores de r2 calculados foram ≥ 0,99 para todos analitos, quando as curvas analíticas foram preparadas em extrato da matriz, demonstrando linearidade satisfatória. Os ensaios de fortificação/recuperação, realizados por dois analistas, em um intervalo de 21 dias, demostraram exatidão e precisão nas concentrações de fortificação de 0,2; 0,5; 1 e 3 μg L-1 (n=7), com percentuais médios de recuperação de 79 a 135% e desvios padrões relativos da repetitividade (DPRr) de até 20%. A reprodutibilidade intralaboratorial (DPRri) mostrou uma repetibilidade < 20% para todos os analitos na maior concentração de fortificação. O método multirresíduo foi validado para determinação de 29 agrotóxicos. O limite de quantificação foi de 0,2 μg L-1 e 0,5 μg L-1 para 10,3% e 89,7% dos agrotóxicos estudados, respectivamente. O método desenvolvido é considerado adequado para determinação de agrotóxicos em água potável e pode ser adotado como alternativa pelos laboratórios que recebem amostras coletadas pelas equipes do VIGIAGUA.Universidade Federal de Santa MariaBrasilQuímicaUFSMPrograma de Pós-Graduação em QuímicaCentro de Ciências Naturais e ExatasPizzutti, Ionara Reginahttp://lattes.cnpq.br/3883506164936996Rosa, Marcelo Barcellos daRoehrs, RafaelReichert, BárbaraBabinski, Paola Jennifer2025-02-20T11:04:45Z2025-02-20T11:04:45Z2024-11-14info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttp://repositorio.ufsm.br/handle/1/34220ark:/26339/001300001bqx6porAttribution-NonCommercial-NoDerivatives 4.0 Internationalinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2025-02-20T11:04:45Zoai:repositorio.ufsm.br:1/34220Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/PUBhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.com||manancial@ufsm.bropendoar:2025-02-20T11:04:45Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
| dc.title.none.fl_str_mv |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras Data analysis of SISAGUA and validation method for pesticides determination in drinking water in order to comply with brazilian legislation |
| title |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras |
| spellingShingle |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras Babinski, Paola Jennifer Monitoramento Multirresíduo SPE LC-MS/MS Monitoring Multiresidue CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
| title_short |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras |
| title_full |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras |
| title_fullStr |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras |
| title_full_unstemmed |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras |
| title_sort |
Análise dos dados do SISAGUA e validação de método para determinação de agrotóxicos em água potável a fim de atender as legislações brasileiras |
| author |
Babinski, Paola Jennifer |
| author_facet |
Babinski, Paola Jennifer |
| author_role |
author |
| dc.contributor.none.fl_str_mv |
Pizzutti, Ionara Regina http://lattes.cnpq.br/3883506164936996 Rosa, Marcelo Barcellos da Roehrs, Rafael Reichert, Bárbara |
| dc.contributor.author.fl_str_mv |
Babinski, Paola Jennifer |
| dc.subject.por.fl_str_mv |
Monitoramento Multirresíduo SPE LC-MS/MS Monitoring Multiresidue CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
| topic |
Monitoramento Multirresíduo SPE LC-MS/MS Monitoring Multiresidue CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
| description |
Water is the foundation of life, playing an essential role in different contexts, which makes it crucial to ensure its availability in adequate quantity and quality. To maintain water potability standards is a challenge because contemporary agriculture use pesticides to meet the global demand for food. However, this practice brings substantial risks to the environment and human health. In Brazil, drinking water potability is regulated by Ordinance GM/MS Nº 888/2021, which establishes the maximum allowable concentrations (MAC) for pesticides and their metabolites. Monitoring of pesticide residues in supply systems is carried out by the National Water Quality Surveillance Program for Human Consumption (VIGIAGUA) and the data is accessible at the Water Quality Surveillance Information System for Human Consumption (SISAGUA). Therefore, the present study aimed to: 1) Evaluate the SISAGUA database related to pesticide residues in water samples from the states of Rio Grande do Sul and São Paulo from 2014 to 2022; 2) To develop and to validate an integrated SPE-LC-MS/MS method for pesticides determination in drinking water. The evaluation of the SISAGUA database revealed that 20 out of the 27 pesticides monitored in the Brazilian water supply systems have results above the MAC, including pesticides banned for agricultural use in Brazil. Aldrin and dieldrin was the most frequently detected pesticide and were found in 40 samples, covering 52% of municipalities, in concentrations between 0.04 and 15 μg L-1. For the extraction of pesticides, the use of C18 and Oasis® HLB cartridges were evaluated, followed by elution by dichloromethane and methanol or ethyl acetate. The best results were achieved using the Oasis® HLB sorbent. The validation study showed that the calculated r2 values were ≥ 0.99 for all analytes, when the analytical curves were prepared in matrix extract, demonstrating satisfactory linearity. The spiking experiments were performed by different analysts, with a 21 days-interval demonstrated accuracy and precision at the spike concentrations of 0.2; 0.5; 1 and 3 μg L-1 (n=7), presenting average recovery percentages of 79 to 135% and relative standard deviations of repeatability (RSDr) of up to 20%. Within-laboratory reproducibility (RSDwR) showed a repeatability < 20% for all analytes at the highest spike concentration. The multiresidue method was validated for the determination of 29 pesticides. The limit of quantification was 0.2 μg L-1 and 0.5 μg L-1 for 10.3% and 89.7% of those studied pesticides, respectively. The developed method is considered suitable for determining pesticides in drinking water and can be adopted as an alternative by laboratories that receive samples collected by VIGIAGUA teams. |
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2024 |
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2024-11-14 2025-02-20T11:04:45Z 2025-02-20T11:04:45Z |
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Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
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Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
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