超高效液相-串联质谱法同时测定蜂蜜中15种喹诺酮类药物残留

Simultaneous determination of 15 quinolones residues in honey by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometric detection

建立了蜂蜜样品中15种喹诺酮类兽药残留的超高效液相色谱-串联质谱检测方法。蜂蜜样品用磷酸盐缓冲溶液溶解提取后,用Oasis HLB固相萃取柱净化,超高效液相-电喷雾串联四级杆质谱检测,外标法定量。测定时用Acquity UPLC BEHC18色谱柱(50 mm×2.1 mm,1.7μm)分离,体积分数0.1%甲酸溶液-乙腈系统梯度洗脱,质谱测定采用多重反应监测(MRM)模式。15种喹诺酮类兽药的检出限均低于或等于1.0 ng/mL,回收率均在78.6%～112.9%范围内,相对标准偏差均在10%范围内。该方法各项指标均能满足国内外各项法规的要求,可用于蜂蜜样品中喹诺酮类药物残留的定量和定性检测。

An ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method was developed for the determination of fifteen quinolones residues in honey.Honey samples were diluted with phosphate buffer solution,then cleaned up with Oasis HLB columns and detected by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometric detection.Quantitation was carried out using an external standard method.Separation of the samples was performed on an acquity UPLC BEH C18 column（50 mm×2.1 mm,1.7 μm） using a gradient solvent system（acetonitrile-0.1% formic acid）.MS/MS was performed with multiple reaction monitoring（MRM） mode.The detection limit of all the 15 quinolones could reach 1.0 ng/mL.The recoveries ranged from 78.6% to 112.9% with relative standard deviations less than 10%.The method is fast,sensitive,with good ruggedness,and all indexes can meet various law and regulation of China and other countries.It′s suitable for quantitative and qualitative analysis of quinolones residues in honey.