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QuEChERS vs QuEChERS-DLLME: Toward an eco-friendly, selective, and sensitive method for levamisole determination in fish

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Autor(es):
de Freitas, Lucas Victor Pereira ; Alponti, Ana Luisa Bigliassi ; Campanharo, Sarah Chagas ; Damaceno, Marina Alves ; da Silva, Agnaldo Fernando Baldo ; Souza, Marilia Cristina de Oliveira ; Assane, Inacio Mateus ; Pilarski, Fabiana ; Sasanya, James Jacob ; Paschoal, Jonas Augusto Rizzato
Número total de Autores: 10
Tipo de documento: Artigo Científico
Fonte: Microchemical Journal; v. 215, p. 11-pg., 2025-08-25.
Resumo

Background: The lack of regulated medicines for aquaculture challenges its expansion and its crucial role in global food security. Reliable bioanalytical methods are essential for monitoring drug residues in food, whether for research on new drugs or surveillance programs that ensure consumer safety. These methods face significant challenges in selectively detecting drugs at residual concentrations (often below 10 mu g kg-1) in complex biological matrices such as muscle, fat, and skin. Since fish fillets consist of two distinct tissues (muscle and skin in natural proportions), the analytical challenges are even greater, requiring highly sensitive and selective approaches. Results: We describe the development of eco-friendly, sensitive, and selective analytical methods for levamisole determination in fish fillets (tilapia, Oreochromis niloticus). The methods involved two sample preparation approaches: one based on a modified QuEChERS method and the other combining QuEChERS with DLLME (Dispersive Liquid-Liquid Microextraction). Both methods were coupled with LC-MS/MS and optimized using multivariate analysis to achieve the best extraction conditions. The proposed methods were validated and found to be selective, precise (CV = 0.6-13 %), and accurate (recovery 98.4-118 %), with linearity ranges of 2-200 mu g kg-1 for QuEChERS and 0.2-20 mu g kg-1 for QuEChERS-DLLME. The QuEChERS-DLLME approach enhanced detectability, achieving the lowest LOQ (0.2 mu g kg-1) reported in the literature for levamisole quantification in fish fillets. The QuEChERS LC-MS/MS method was successfully applied to incurred tilapia samples treated with levamisole. Significance: Despite the well-recognized advantages of QuEChERS-based methods, known for their versatility and robustness, and DLLME-based methods, valued for their high selectivity and sensitivity, to the best of our knowledge, the combination of QuEChERS and DLLME for levamisole determination in fish samples has not been reported. Therefore, this study may serve as a valuable reference to promoting the adoption of this combined approach for other applications. (AU)

Processo FAPESP: 21/11996-6 - Avaliação de procedimentos de incorporação do levamisol na ração de peixes
Beneficiário:Ana Luísa Bigliassi Alponti
Modalidade de apoio: Bolsas no Brasil - Iniciação Científica
Processo FAPESP: 21/03294-1 - Estudos para o uso de levamisol na Aquicultura: métodos analíticos; incorporação na ração; depleção residual; e estimativa de período de carência
Beneficiário:Lucas Victor Pereira de Freitas
Modalidade de apoio: Bolsas no Brasil - Doutorado
Processo FAPESP: 21/08152-0 - Desafio do uso de medicamentos na piscicultura no contexto One Health: avaliação da eficácia, segurança e análise de risco
Beneficiário:Jonas Augusto Rizzato Paschoal
Modalidade de apoio: Auxílio à Pesquisa - Temático