RESUMO
Hainanmycin is a new veterinary polyether antibiotic and has few sensitive analytical method in present days. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) relying on multiple reaction monitoring (MRM) detection was developed for analysis of hainanmycin in animal feed. Feed samples were extracted with ethyl acetate and purified by two steps of liquid-liquid extraction (LLE) to get rid of water solvable matrix and lipids one by one. The final simple was analyzed by LC-MS/MS. The LC mobile phase was composed of 0.1% aqueous formic acid and 0.1% formic acidified acetonitrile by gradient elution. Average recoveries ranged from 74.22% to 87.85%, as determined by spiking with 2.0 (LOQ) â¼2500µgkg-1 of hainanmycin. The inter-day and intra-day coefficient of variation was 9.21% to 11.77% and 7.67% to 13.49%, respectively. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.36µgkg-1 and 2.0µgkg-1, respectively.
Assuntos
Ração Animal/análise , Cromatografia Líquida/métodos , Éteres/análise , Ionóforos/análise , Extração Líquido-Líquido/métodos , Espectrometria de Massas em Tandem/métodos , Éteres/química , Éteres/isolamento & purificação , Ionóforos/química , Ionóforos/isolamento & purificação , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos TestesRESUMO
An ultra-performance liquid chromatography with tandem mass spectrometric detection (UPLC-MS/MS) method was developed for the detection of flunixin residues in rabbit tissues. The samples were extracted with acidic acetonitrile, defatted with n-hexane, and then purified by HLB solid-phase extraction cartridge. Analysis was carried out on UPLC-ESI-MS/MS working with multiple reaction monitoring (MRM) mode. The limits of detection (LODs) of the method were 0.3-0.8µgkg(-1) and limits of quantification (LOQs) were 1.0-3.0µgkg(-1) in rabbit tissues, respectively. In all fortified samples at a concentration range of 1.0-300.0µgkg(-1), mean recoveries were 61.7-115.7% with relative standard deviations (RSDs) below 16%. Residue depletion of flunixin in rabbit was conducted after oral administration at a dose of 5mgkg(-1) of body weight. The average concentrations for flunixin measured 2h post-administration in kidney and intestine were significantly higher than in liver, heart and muscle. The concentrations for flunixin in all rabbit tissues were below the LOD or not detected in all tissues after 96h administration of drug. A minimum withdrawal time of 21h was indicated for residue levels in heart, liver, kidney, intestine and muscle below the maximum residue limits (MRLs).