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Development and validation of an LC-MS/MS method for analysing doxycycline in medicated fish-feed and evaluation of top-coating procedures

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Autor(es):
Damaceno, Marina Alves ; de Freitas, Lucas Victor Pereira ; Campanharo, Sarah Chagas ; da Silva, Agnaldo fernando Baldo ; Sasanya, James Jacob ; Paschoal, Jonas Augusto Rizzato
Número total de Autores: 6
Tipo de documento: Artigo Científico
Fonte: Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure; v. N/A, p. 12-pg., 2026-01-19.
Resumo

Antimicrobials are widely used to control diseases in fish farming. Irregular use of these substances can reduce treatment efficacy and contaminate aquatic environments, promoting the emergence and spread of antimicrobial-resistant bacteria. Doxycycline, a broad-spectrum antimicrobial active against both Gram-positive and Gram-negative bacteria, is authorised for use in aquaculture in several countries and represents a promising therapeutic option. However, to date, no studies have investigated its incorporation into fish feed or its potential to leach into the environment. This study aimed to develop, optimise, and validate an LC-MS/MS method to detect doxycycline in medicated feed and to evaluate top-coating procedures to ensure treatment efficacy while minimising leaching into the environment. The LC-MS/MS method was optimised using a Plackett-Burman design to determine the optimal sample extraction conditions and, subsequently, validated, demonstrating selectivity, precision (CV < 3.5%), accuracy (recovery of 98.4-102%), and linearity (R-2 > 0.99, 1.6-8.3 g kg(-1)). Two top-coating procedures using ethyl cellulose and gelatine polymers were evaluated; both achieved high incorporation efficiency (70%) and homogeneous drug distribution within feed pellets (CV < 2%). Leaching-tests showed that the top-coatings effectively retained doxycycline, with leaching rates below 5% after 15 min of immersion. Overall, these approaches may enhance treatment efficacy and mitigate the environmental impact, promoting the responsible use of antimicrobials in fish farming in accordance with the One Health concept. (AU)

Processo FAPESP: 25/09150-2 - Avaliação Integrada da Dinâmica Ambiental e Toxicológica do Levamisol na Piscicultura: Uma Abordagem One Health
Beneficiário:Lucas Victor Pereira de Freitas
Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado
Processo FAPESP: 19/06159-8 - Estudos para o uso seguro de eritromicina e doxiciclina em peixes de importância comercial nacional
Beneficiário:Jonas Augusto Rizzato Paschoal
Modalidade de apoio: Auxílio à Pesquisa - Regular
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