Simultaneous Determination of Four Nitrofuran Antibiotics Residues in Feedstuff by High Performance Liquid Chromatography-Tandem Mass Spectrometry

KeyWord:liquid chromatography-tandem mass spectrometry£¨LC-MS/MS£©  positive and negative switching scan mode  nitrofuran antibiotics  feedstuff

Abstract:

      A method was developed for the determination of furazolidone£¨FZD£©£¬furaltadone£¨FTD£©£¬furacilin£¨NFZ£©and nitrofurantoin£¨NFT£© residues in feedstuff by isotope dillution high performance liquid chromatography-tandem mass spectrometry.After homogenization£¬samples were extracted with acetonitrile.After centrifugation£¬the extract was evaporated to dryness with nitrogen at 40¡æ£¬and redissolved with acetonitrile-0.05%ammonium acetate solution.The solution was defatted with hexane and cleaned up with neutral alumina solid phase extraction cartridge.The targeted compounds were seperated on a Sunfire C18£¨150 mm¡Á2.1 mm£¬5 ¦Ìm£© column by using methanol-0.05% ammonium acetate as mobile phase£¬and detected with electrospray ionization£¨ESI£© under positive and negative switching scan mode£¬ in which negative scan mode was used for NFZ and NFT,respectively£¬and positive scan mode was used for FZD and FTD.The detection limits were 2.0 ¦Ìg/kg for FZD and NFT and 3.0 ¦Ìg/kg for FTD and NFZ,respectively.The quantitation limits were 5.0 ¦Ìg/L for FZD and NFT£¬and 10.0 ¦Ìg/kg for FTD and NFZ,respectively.The linear ranges of the target compounds ranged from 5.0 ¦Ìg/L to 100.0 ¦Ìg/L with correlation coefficients greater than 0.99.The recoveries of four compounds in spiked feed for tilapia were in the range of 78%-107% with relative standard deviations£¨RSDs£© less than 12%.The method is rapid and accurate£¬and is suitable for the detection of four nitrofuran drugs in feedstuff.