Abstract:In order to simultaneously detect and quantify the residues of seven benzimidazole and two nitroimidazole drugs in multiple matrices, a method for the simultaneous detection of triclabendazole ketone, mebendazole, hydroxymebendazole, amino mebendazole, fenbendazole, oxfendazole, oxfendazole sulfone, ronidazole and tinidazole residues in animal-derived foods was established by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Samples were pretreated with hydroxylamine hydrochloride solution to protect triclabendazolone, then extracted with acidic acetonitrile, purified on a PRiME HLB solid phase extraction column, separated on a C18 Core shell column with gradient elution using methanol-0.1% formic acid in water as mobile phase. Ionization was performed in electrospray positive ion mode, detection was carried out in selected reaction monitoring mode (Selected Reaction Monitoring, SRM), and quantification was achieved by isotope internal standard method. The seven benzimidazoles showed good linearity in the range of 10–400 ng·mL-1 (correlation coefficients R2 > 0.99) with a limit of quantification (LOQ) of 10 μg·kg-1. The two nitroimidazoles showed good linearity in the range of 1–40 ng·mL-1 (R2 > 0.99) with an LOQ of 1.0 μg·kg-1. Spiked recovery tests were conducted in pork, fish, egg, milk and honey at three levels (1LOQ、2LOQ and 10LOQ). The average recoveries ranged from 71.3% to 106.4%, with relative standard deviations (RSDs) of 0.6%–9.2%. This method features simple operation, high sensitivity and a wide matrix coverage range. It enables the simultaneous detection of residues of multiple benzimidazoles and nitroimidazoles in animal-derived foods, meets the stringent international residue limits, and provides reliable technical support for the food safety supervision of import and export commodities.