应用超高效液相色谱串联质谱建立鸡蛋中加雷沙星、曲伐沙星、莫西沙星、奥比沙星、吉米沙星、加替沙星、培氟沙星和环丙沙星等22种喹诺酮类药物残留检测方法。样品经过2%甲酸乙腈提取、正己烷分步去脂，Oasis HLB柱净化后，经Acquity UPLC BEH Shield RP18（100 mm×2.1 mm，1.7 μm）分离，以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱，双通道MRM信号采集模式，22种喹诺酮类药物能在11 min完好分离，方法的最低定量限均低于1.0 μg/kg，在2.0~100.0 μg/L浓度范围内，22种喹诺酮类药物线性良好，相关系数均在0.99以上；通过2、10、20 g/kg三个浓度的加标回收实验表明，回收率为60.1%~96.2%，RSD%值为1.44%~11.1%。该方法相比现有国标检测药物种类多，新型药物多，对更全面筛查和确证鸡蛋中喹诺酮类药物残留，防范非法添加造成安全隐患具有一定的参考价值。

A multiresidue method for the determination of twenty-two quinolone residues (garenoxacin, trovafloxacin, moxifloxacin, orbifloxacin, gemifloxacin, gatifloxacin, pefloxacin, ciprofloxacin, etc.) in eggs was developed based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). In this method, the analytes were extracted using acidified (2%) acetonitrile, degreased by n-hexane, and purified through an Oasis HLB SPE column. The twenty-two quinolones were separated on an Acquity UPLC BEH Shield RP18 column (100 mm×2.1 mm, 1.7 μm), using methanol and 0.1% formic acid as the mobile phases for gradient elution. The signals were acquired through the dual-channel multiple reaction monitoring (MRM) mode. All analytes could be well separated by using a gradient program of 11 minutes. The calibration curves of the twenty-two quinolones showed good linearity in the concentration range of 2.0~100.0 μg/L (r>0.99), and the limits of quantitation were all less than 1.0 μg/kg. The recoveries of the 2, 10 and 20 μg/kg spiked samples ranged from 60.1% to 96.2%, with RSDs of 1.44%~11.1%. Compared with the existing national standard, this new method has the advantage of detecting more types of quinolone drugs, especially the new ones. The new method has a certain reference value for a more comprehensive screening and identification of quinolone residues in eggs and prevention of illegal additions.

十二五国家科技支撑计划项目（2014BAD13B05）；河南省重点科技攻关项目（162102210107）