液相色谱-串联质谱法测定鸡蛋中的喹诺酮类和四环素类抗生素

Determination of Quinolones and Tetracyclines in Egg by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

应用液相色谱-串联质谱法技术,建立鸡肉中喹诺酮类和四环素类抗生素的检测方法,并对宁夏地区市售鸡蛋进行分析。鸡蛋样品经EDTA-Mcllvaine缓冲溶液超声提取,玻璃纤维滤膜过滤,HLB固相萃取柱净化,乙腈-0.1%甲酸水溶液为流动相,用Waters Atlantis T_3色谱柱分离,以电喷雾正离子模式进行质谱测定。三个加标水平下喹诺酮类抗生素回收率为80.0%～114.0%,相对标准偏差小于12.0%,检出限(S/N=3)为0.2μg/kg,定量限(S/N=10)为0.8μg/kg;四环素类抗生素的平均回收率为84.5%～110.0%,相对标准偏差小于12.0%,检出限(S/N=3)为0.2μg/kg,定量限(S/N=10)为0.8μg/kg。该方法操作快速简单、重现性好,可用于鸡蛋中喹诺酮类和四环素类抗生素的检测。

To develop a rapid method for determination of quinolones and tetracyclines in egg by liquid chromatography tandem mass spectrometry(LC-MS/MS) and provide analytical methodology for the egg in Ningxia province,samples of eggs were ultrasonically extracted by EDTA-Mcllvaine buffer solution,filtrated by glass fiber membrane and then cleaned up by HLB column. Quinolones and tetracyclines were separated on Waters Atlantis T3 chromatographic column with mobile phase of methanol-0.1% formic acid on gradientelution. Ionized by atmospheric pressure chemicalionization,the quinolones and tetracyclines were qualified and quantified by mass spectrometry. Average recoveries of quinolones and tetracyclines in egg at three spiked levels were 80.0% ~114.0% and 84.5% ~110.0% with relative standard deviations less than 12.0%,respectively.The limit of detection(LOD) and the limit of quantitation(LOQ) for the whole method were 0.2 μg/kg and 0.8 μg/kg,respectively.The method was accurate,reliable,and could be used as a quality control method for quinolones and tetracyclines in egg.