Quantification of 8-α-hydroxy-mutilin as marker residue for tiamulin in rabbit tissues by high-performance liquid chromatography-mass spectrometry.

摘要: For the first time, a sensitive and specific method was developed fully validated for quantification of EU marker residue tiamulin, 8-α-hydroxy-mutilin, in rabbit muscle liver tissues using liquid chromatography combined with positive heated electrospray ionization triple quadrupole mass spectrometry. The spectrometer operated selected reaction monitoring (SRM) mode selection [M + H]+ ion both quadrupoles 1 3, resulting SRM transition m/z 337.25 > quantification. Chromatography performed Hypersil Gold C18 column gradient elution program water methanol as mobile phases. sample preparation procedure analysis 8-α-hydroxy-mutilin samples consisted three main steps: (1) extraction tissue matrix 0.1 N hydrochloric acid/acetone (50/50, v/v), (2) hydrolysis tiamulin metabolites to alkaline medium at 45 °C, (3) liquid–liquid acidic ethyl acetate. This is presenting results, encompassing linearity 50 2,000 μg/kg, within-run between-run accuracy precision, limit (50 μg/kg tissues), detection (muscle, 11.9 μg/kg; liver, 20.6 μg/kg), recovery 66.2 %; 75.5 %), signal suppression enhancement 51.7 43.3 carryover, applicability practicability, stability during storage analysis. novel therefore enough be used depletion studies rabbits food safety respect MRL compliance residues.