Optimization and validation method to evaluate the residues of β-lactams and tetracyclines in kidney tissue by UPLC-MS/MS.
Autor: | de Almeida MP; Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil., Rezende CP; Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil., Ferreira FD; Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil., de Souza LF; Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n, Pedro Leopoldo, MG CEP 33600-000, Brazil., de Assis DC; Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 30123-970, Brazil., de Figueiredo TC; Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 30123-970, Brazil., de Oliveira Leite M; Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 30123-970, Brazil., de Vasconcelos Cançado S; 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. |
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Jazyk: | angličtina |
Zdroj: | Talanta [Talanta] 2015 Nov 01; Vol. 144, pp. 922-32. Date of Electronic Publication: 2015 Jul 17. |
DOI: | 10.1016/j.talanta.2015.07.048 |
Abstrakt: | 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. (Copyright © 2015 Elsevier B.V. All rights reserved.) |
Databáze: | MEDLINE |
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