title: Optimization and validation method to evaluate the residues of β-lactams and tetracyclines in kidney tissue by UPLC-MS/MS.
abstract: Methods are validated by a process that defines the analytical requirements and confirms that the investigated method is capable of performing consistently. A quantitative and confirmatory method for determining the presence of β-lactam and tetracycline multiresidues in avian, bovine, equine, and swine kidney tissues using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed, optimized, and validated. Analytes were extracted from the kidneys by a mixture of water and acetonitrile, and the extract was then purified with hexane and C18 (dispersive phase). The method was evaluated by the following parameters: linearity, matrix effect, specificity, decision limits (CCα), detection capability (CCβ), accuracy, precision, trueness, limits of detection (LOD), limits of quantification (LOQ), and robustness. The validated method presented a broad linear study range and significant matrix effect. The limit of detection (LOD) was defined from 2.5 to 25.0 µg kg(-1), and the limit of quantification (LOQ) was defined from 5.0 to 50.0 µg kg(-1) for individual analytes. The resultant recovery values ranged from 98.1% to 107.3% in repeatability conditions and from 95.2% to 106% under intralaboratory reproducibility conditions for the studied analytes. It was concluded that the performance parameters demonstrated total method adequacy for detecting and quantifying β-lactam and tetracycline residues in swine, equine, bovine, and avian kidneys.
authors.affiliation: Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil.
authors.forename: Marcos Pego
authors.initials: MP
authors.lastname: de Almeida
authors.affiliation: Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil.
authors.forename: Cristiana Perdigão
authors.initials: CP
authors.lastname: Rezende
authors.affiliation: Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil.
authors.forename: Flavia Domingues
authors.initials: FD
authors.lastname: Ferreira
authors.affiliation: Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil.
authors.forename: Leonardo Francisco
authors.initials: LF
authors.lastname: de Souza
authors.affiliation: Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 30123-970, Brazil.
authors.forename: Débora Cristina Sampaio
authors.initials: DC
authors.lastname: de Assis
authors.affiliation: Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 30123-970, Brazil.
authors.forename: Tadeu Chaves
authors.initials: TC
authors.lastname: de Figueiredo
authors.affiliation: Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 30123-970, Brazil.
authors.forename: Mônica
authors.initials: M
authors.lastname: de Oliveira Leite
authors.affiliation: Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 30123-970, Brazil. Electronic address: silvanavc@ufmg.br.
authors.forename: Silvana
authors.initials: S
authors.lastname: de Vasconcelos Cançado
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D001717:Birds; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods; D006736:Horses; D007668:Kidney / Q000737:chemistry*; D057230:Limit of Detection; D015203:Reproducibility of Results; D013552:Swine; D053719:Tandem Mass Spectrometry; D013754:Tetracyclines / Q000032:analysis*; D047090:beta-Lactams / Q000032:analysis*
chemical_list: D000900:Anti-Bacterial Agents; D013754:Tetracyclines; D047090:beta-Lactams
keywords: Kidney; Tetracycline; UPLC–MS/MS; Validation; β-lactam