DEVELOPMENT AND VALIDATION OF ANALYTICAL METHODS FOR MULTIRESIDUE  DETERMINATION OF PESTICIDES IN ENVIRONMENTAL MATRICES

Adilson Correia Goulart; Simone Machado Goulart; Anizio Márcio de Faria

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Trabalho

Título do Trabalho

DEVELOPMENT AND VALIDATION OF ANALYTICAL METHODS FOR MULTIRESIDUE DETERMINATION OF PESTICIDES IN ENVIRONMENTAL MATRICES

Autores

Adilson Correia Goulart
Simone Machado Goulart
Anizio Márcio de Faria

Modalidade

Resumo

Área temática

Contaminantes emergentes e Agrotóxicos

Data de Publicação

15/04/2024

País da Publicação

Brasil

Idioma da Publicação

Português

Página do Trabalho

https://www.even3.com.br/anais/xv-laseac-x-enqamb-2024i/775396-development-and-validation-of-analytical-methods-for-multiresidue--determination-of-pesticides-in-environmental-m

ISBN

978-65-272-0404-6

Palavras-Chave

solid-liquid extraction, liquid-liquid extraction, low-temperature partitioning, analytical ecoscale, environmental contamination.

Resumo

The principal purpose of using pesticides is to protect crops from the harmful actions of beings considered harmful to this environment. However, a considerable number of pesticides reach non-target beings and environmental compartments.1 Soil, surface, and groundwater are the principal destinations for pesticide residues. Therefore, studies aimed at developing analytical methods for determining pesticides are essential.2 Therefore, the objective of this study was to develop and validate two analytical methods for determining the pesticides carbendazim, thiodicarb, diuron, fipronil, and chlorpyrifos in soil and water matrices. Solid-liquid extraction (SLE) and liquid-liquid extraction (LLE), followed by low-temperature partition (LTP), were the sample preparation methods chosen. These methods have been used to determine various pesticides in different matrices. The analytical technique for the separation, identification, and quantification of the analytes was high-performance liquid chromatography with UV detection. In optimizing the methods, a 23-factorial design was applied, evaluating the effects of the factors: volume of acetonitrile (4 or 6 mL), vortexing time (1 or 2 min), and addition of NaCl to evaluate the effect of ionic strength. In all optimization tests, average analyte recovery percentages higher than 85% were obtained in both matrices analyzed, indicating the applicability of the methods. The effects of the factorial planning factors were evaluated by the t-test, with 5% significance and 95% confidence, suggesting that 6 mL of acetonitrile, 1 min of agitation, and the absence of NaCl are more favorable conditions for the extraction of analytes in the matrices studied. The validation study showed good selectivity, good linearity (R2>0.99), and accuracy at three concentration levels (recovery rates between 85-110%) for both methods. The accuracies of the two methods showed relative standard deviations (RSD) <13.20% and low limits of detection and quantification, according to guidelines established by the European Community validation guide Sante/11312/2021.3 The method robustness was evaluated by applying the Youden and Steiner test. All seven parameters analyzed indicated variations of less than 12% in the pesticide recovery rates, keeping it in the range of 70-120%. The greenness of the proposed methods was evaluated by the analytical ecoscale, reaching seventy-eight points, and classifying the ESL/ELL-PBT methods as excellent greenness methods. Therefore, the developed and validated ESL/ELL-PBT methods constitute excellent eco-friendly alternatives for the determination and monitoring of carbendazim, thiodicarb, diuron, fipronil, and chlorpyrifos residues in water and soil samples. References: 1Dugan, S.T.; et al. Sci. Total Environ., 901 (2023) 165892. 2Tudi, M.; et al. Int. J. Environ. Res. Pub. Health 18 (2021) 1112. 3Document SANTE/11312/2021.

Título do Evento: XV LASEAC - X ENQAmb 2024.
Cidade do Evento: Ouro Preto
Título dos Anais do Evento: Anais do XV LASEAC (Latin American Symposium on Environmental Analytical Chemistry) & X ENQAmb (Encontro Nacional de Química Ambiental)
Nome da Editora: Even3
Meio de Divulgação: Meio Digital

Como citar

GOULART, Adilson Correia; GOULART, Simone Machado; FARIA, Anizio Márcio de. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHODS FOR MULTIRESIDUE DETERMINATION OF PESTICIDES IN ENVIRONMENTAL MATRICES.. In: . Disponível em: https//www.even3.com.br/anais/xv-laseac-x-enqamb-2024i/775396-DEVELOPMENT-AND-VALIDATION-OF-ANALYTICAL-METHODS-FOR-MULTIRESIDUE--DETERMINATION-OF-PESTICIDES-IN-ENVIRONMENTAL-M. Acesso em: 02/06/2025