超高效液相色谱-串联质谱法测定动物源食品中16种喹诺酮类药物的残留

Determination of 16 Quinolones Residues in Animal Derived Food by Ultra High Performance Liquid Chromatography- Tandem Mass Spectrometry

目的:建立动物源食品中16种喹诺酮类药物的超高效液相色谱-串联质谱测定方法,对日常生活中动物源食品样品进行检测。方法:样品用EDTA-Mcllvaine缓冲液超声提取,提取液经HLB(200 mg/6 mL)固相萃取小柱净化浓缩,采用UPLC-MS/MS多反应监测模式、电喷雾串联四极杆质谱进行测定,外标法定量。结果:16种喹诺酮类药物在2~100 ng·mL^(-1)线性关系良好,相关系数R> 0.991。16种喹诺酮类药物的检出限(S/N=3)为0.5~1.0μg·kg^(-1),定量限(S/N=10)为1.6~3.5μg·kg^(-1)。16种目标化合物在3个加标水平下的平均回收率在81.9%~106.8%,相对标准偏差为1.3%~12.8%。结论:本方法重现性好、灵敏度高,适用于动物源食品中16种喹诺酮类药残留的检测。

Objective:To establish an ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of 16 quinolones in animal-derived foods,and to detect animal derived food samples in daily life.Method:The sample was extracted with EDTA Mcllvaine buffer solution by ultrasonic extraction,and the extract was purified and concentrated by HLB(200 mg/6 mL)solid phase extraction column.UPLCMS/MS multi reaction monitoring mode and electrospray spray tandem quadrupole mass spectrometry were used for determination,and external standard method was used for quantification.Result:The 16 quinolones had a good linear relationship at 2~100 ng·mL^(-1),and the correlation coefficient R>0.991.The limit of detection(S/N=3)of 16 quinolones were 0.5~1.0μg·kg^(-1),and the limit of quantification(S/N=10)were 1.6~3.5μg·kg^(-1).The average recoveries of 16 target compounds at three spiked levels were 81.9%~106.8%,and the relative standard deviations were 1.3%~12.8%.Conclusion:This method has good reproducibility and high sensitivity,and is suitable for the detection of 16 quinolones residues in animal-derived food.