关键词: 超高效液相色谱-四级杆-质谱, 丁香酚, 水产品

Abstract: Objective To establish a method for detecting residual eugenolin aquatic products using ultra high performance liquid chromatography quadrupole mass spectrometry. Methods Fish and shrimp meat samples were ultrasonically extracted with acetonitrile at room temperature,purified by HLB solid-phase extraction column,enriched concentrated by nitrogen flushing,and then diluted with 25% methanol aqueous solution and centrifuged through a membrane. Gradient elution was performed using methanol-0.01% ammonia solution as the mobile phase,and separated by Kromasil Eternity XT-2.5-PhenylHexy（2.1 mm×100 mm,1.7 μm） chromatographic column. The detection was performed in multiple reaction monitoring（MRM） mode with negative electrospray ionization and quantified by internal standard method. Results The linear relationship of eugenol was good within the range of 2.0-200 μg/L（r≥0.999）. The detection limit of the method was 1.0 μg/kg,and the quantification limit was 2.5 μg/kg. The average recoveries（n=6） at low,medium,and high spiked levels（2.5,7.5,and 100 μg/kg） was between 98.0% and 107.0%,and the precision（n=6） was between 1.70% and 7.07%. Using this method,30 fish and shrimp samples were tested with a detection rate of 40%. The detection rate in fish products was 75%,and the detection rate in shrimp products was 0. Conclusion The established method is simple and fast to operate,and the quantitative results are accurate and reliable,which can achieve the detection of eugenol in aquatic products in a short period of time.

Key words: Ultra high performance liquid chromatography coupled withquadrupole mass spectrometry, Eugenol, Aquatic product