超高效液相色谱-串联三重四级质谱法测定动物源性食品中的喹诺酮类和四环素类残留

Determination of quinolones and tetracyclines residues in animal-origin foods by ultra performance liquid chromatography-tandem triple quaternary mass spectrometry

目的建立一种超高效液相色谱-串联三重四级质谱法测定动物源性食品中6种喹诺酮类(氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、环丙沙星、恩诺沙星)和2种四环素类(强力霉素、土霉素)的残留量。方法样品用0.1 mol/L EDTA-Mcllvaine缓冲液提取后,经过滤和离心后,上清液经HLB固相萃取柱净化,电喷雾正离子模式测定,用外标法定量。结果氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、环丙沙星、恩诺沙星、强力霉素、土霉素在1μg/L~100μg/L浓度内与峰面积具有良好的线性关系,相关系数>0.994,8种抗生素在1.0μg/kg、5.0μg/kg、50.0μg/kg 3个水平加标下,回收率为80.5%~96.2%,相对标准偏差(RSD)为1.95%~4.68%。方法的检出限为0.191μg/kg~0.978μg/kg。结论该方法具有灵敏度高、通用性强、准确度高、稳定性好等优点,满足测定动物源性食品中喹诺酮类和四环素类残留的检测要求。

Objective A method for the determination of 6 kinds of quinolones and 2 kinds of tetracyclines residues in animal-origin foods by ultra performance liquid chromatography-tandem triple quaternary mass spectrometry(UPLC-MS/MS)was established.Methods The target analytes were extracted from the samples by 0.1 mol/L EDTA-Mcllvaine buffer extraction solution and purified by HLB solid phase extraction cartridge,and analyzed by UPLC-MS/MS,with positive electrospray ionization(ESI+)in multiple reaction monitoring(MRM)mode,and quantified by external standard method.Results The calibration curves of 8 antibiotics showed good linearities in the range of 1μg/L-100μg/L with correlation coefficients(r)greater than 0.994.The recoveries of 8 antibiotics were between 80.5%-96.2%at the spiked levels of 1.0μg/kg,5.0μg/kg,and50.0μg/kg,and the relative standard deviation was between 1.95%-4.68%.The limits of detection of the method were in the range of 0.191μg/kg-0.978μg/kg.Conclusion The method had many advantages such as high sensitivity,high accuracy,strong versatility,good stability and was suitable for determination of quinolones and tetracyclines residues in animal-origin foods.