Determination of Ciguatoxin Residues in Deep Sea Fish by Auto-SPE/High Performance Liquid Chromatography-Tandem Mass Spectrometry

KeyWord:high performance liquid chromatography-tandem mass spectrometry£¨HPLC-MS/MS£©  ciguatoxin  deep sea fish

Abstract:

      A high performance liquid chromatography-tandem mass spectrometric£¨HPLC-MS/MS£© method was established for the determination of ciguatoxin in deep sea fish£®The residues in fish were extracted with methanol-hexyl hydride£¨4¡Ã1£©£¬and purified by an HLB SPE column.The detection of ciguatoxin was performed by mass spectrometry with electrospray in positive ionization mode and multiple reaction monitoring£¨MRM£© mode.No significant matrix effect was found for the spiked samples after purification£®The recoveries of ciguatoxin in food were in the range of 70%-84% at spiked levels of 0.01-0.1 ¦Ìg/kg£®The relative standard deviations£¨RSDs£© were less than 7%£®The limits of detection£¨LOD£© and the limits of quantitation£¨LOQs£© were 0.01 ¦Ìg/kg and 0.02 ¦Ìg/kg£¬respectively£®This method was simple,rapid and reliable,and could meet the requirement for determination of ciguatoxin in deep sea fish£®