Determinação multirresíduo de agrotóxicos e medicamentos veterinários em carne bovina empregando método QuEChERSER e UHPLC-MS/MS

• Ano de defesa: 2026
• Autor(a) principal: Samborski, Theo
• Tipo de documento: Dissertação
• Tipo de acesso: Acesso aberto
• Idioma: por
• Instituição de defesa: Universidade Federal de Santa Maria; Brasil; UFSM; Programa de Pós-Graduação em Química; Centro de Ciências Naturais e Exatas
• Palavras-chave em Português: Carne bovina; Multirresíduo; QuEChERSER; UHPLC-MS/MS; Validação; Beef; Multiresidue; Validation; CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
• Link de acesso: http://repositorio.ufsm.br/handle/1/38455

Beef is widely consumed in Brazil and worldwide, serving as a major source of high-biological-value protein. However, the presence of pesticide residues and veterinary drug residues in this foodstuff raises significant concerns regarding food safety and public health. This necessitates the development of sensitive, selective, and reliable multiresidue analytical methods capable of combining high analytical throughput with an appropriate analysis frequency in routine laboratories. In this context, the present study aimed to develop and validate an analytical method for the simultaneous determination of pesticide and veterinary drug residues in bovine muscle using UHPLC-MS/MS. Different sample preparation strategies were evaluated, including variations in extraction conditions and cleanup procedures, with the goal of minimizing matrix effects, maximizing analyte recovery, and maintaining suitable analytical throughput and sample analysis frequency for routine applications. The validated method employed 2 g of bovine muscle sample, extracted with ACN:H₂O (4:1, v/v) under agitation for 10 min, followed by cleanup on an EMR-Lipid® cartridge (40 mg). The extract was then diluted (1:4 in water), centrifuged, and filtered prior to instrumental analysis. Chromatographic separation was performed by UHPLC-MS/MS in selected reaction monitoring (SRM) mode, using gradient elution with a mobile phase consisting of (A) water containing 5 mmol L⁻¹ ammonium formate and 0.1% (v/v) formic acid, and (B) acetonitrile with the same modifiers. The method was validated in accordance with Commission Implementing Regulation (EU) 2021/808, demonstrating adequate performance in terms of selectivity, matrix effects, linearity, trueness, and precision. The decision limit (CCα) values were compatible with the respective maximum residue limits (MRLs) established, confirming the method's fitness for purpose in official control applications. Application of the method to real bovine muscle samples from Rio Grande do Sul revealed no detectable levels of the target compounds above their limits of quantification. Thus, the developed method proved to be robust, rapid, and reliable for the multiresidue determination of pesticides and veterinary drugs in bovine meat.