关键词: 固相萃取, 超高效液相色谱-串联质谱法, 兽药多残留, 动物源性食品

Abstract: An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with solid phase microextraction method was established for the simultaneous determination of 72 veterinary drugs including sulfanilamide, quinolone, glucocorticoid, macrolides, beta-agonist, steroid hormone, tetracycline, penicillin, chloramphenicol and beta-lactam in pork, fish and shrimp samples. Samples were extracted by 80% (V/V) acetonitrile in water, followed by cleanup of the extracts through a Prime HLB solid phase extraction column directly without activation. Separation was performed on a C18 column and the eluates were detected by multiple reaction monitoring scanning with electronic spray ionization. An external standard method was applied for quantification. The limits of quantitation (LOQ) for 72 veterinary drugs were in the range of 0.5 to 5 μg/kg. Recoveries from different food matrices were from 75.6% to 122.3% with relative standard deviations between 0.6% and 10.7%. This method was significantly efficient in the determination of multiple veterinary drugs and suitable for rapid multiresidual analysis of veterinary drugs in handling of food safety emergencies.

Key words: solid phase extraction, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), veterinary drug multiresidues, animal-derived food