Optimization and validation method to evaluate the residues of β-lactams and tetracyclines in kidney tissue by UPLC–MS/MS

• Published in: Talanta (Oxford) 2015-11, Vol.144, p.922-932
• Main Authors: de Almeida, Marcos Pego, Rezende, Cristiana Perdigão, Ferreira, Flavia Domingues, de Souza, Leonardo Francisco, de Assis, Débora Cristina Sampaio, de Figueiredo, Tadeu Chaves, de Oliveira Leite, Mônica, de Vasconcelos Cançado, Silvana
• Format: Article
• Language: English
• Subjects: Animals; Anti-Bacterial Agents - analysis; beta-Lactams - analysis; Birds; Cattle; Chromatography, Liquid - methods; Horses; Kidney; Kidney - chemistry; Limit of Detection; Reproducibility of Results; Swine; Tandem Mass Spectrometry; Tetracycline; Tetracyclines - analysis; UPLC–MS/MS; Validation; β-lactam
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2015.07.048

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 25.0µgkg−1, and the limit of quantification (LOQ) was defined from 5.0 to 50.0µgkg−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. [Display omitted] •UPLC–MS/MS method was validated for the study of residues of antibiotics.•Method is suitable for analyses of β-lactam and tetracycline residues in kidney.•Method is apt for detecting residues in swine, equine, bovine, and avian kidneys.•The method has the ability to analyze several residues in a single analytical run.