Validated method for determination of ultra-trace closantel residues in bovine tissues and milk by solid-phase extraction and liquid chromatography–electrospray ionization-tandem mass spectrometry

Abstract

A liquid chromatographic–electrospray ionisation-tandem mass spectrometry method (LC–ESI-MS/MS) with solid extraction was developed and validated for the detection and determination of closantel residues in bovine tissues and milk. An acetonitrile–acetone mixture (80:20, v/v) was used for one-stage extraction of closantel residues in bovine tissues and milk samples, and the extract was cleaned by solid phase extraction with Oasis MAX cartridges. The mass spectrometer was operated in multiple reactions monitoring mode with negative electrospray interface. The limits of detection in different matrices were in the range of 0.008–0.009 μg/kg. The overall recoveries for bovine muscle, liver, kidney and milk samples spiked at four levels including MRL were in the range of 76.0–94.3%. The overall relative standard deviations were in the range of 3.57–8.61%. The linearity is satisfactory with a correlation coefficient ( r 2) of 0.9913–0.9987 at both concentration ranges of 0.02–100 μg/kg and 200–5000 μg/kg. The method is capable of identifying closantel residues at ≥0.02 μg/kg levels and was applied in the determination of closantel residues in animal origin foods.