摘要
目的建立鸡蛋中喹诺酮类和四环素类药物残留量的超高效液相色谱-质谱同时检测方法。方法样品用EDTA-Mcllvaaine提取液超声提取,经过滤和离心后,上清液经HLB固相萃取柱净化。采用C18色谱柱(2.1 mm×100 mm,1.7μm)分离,以乙腈-0.2%甲酸水溶液梯度洗脱,多反应监测模式(MRM)测定,外标法定量。结果 21种喹诺酮类和四环素类药物在2μg/kg^100μg/kg浓度内线性关系良好(r>0.994 0),方法的检出限为0.5μg/kg^2.0μg/kg,21种抗生素在鸡蛋中的加标回收率为79.5%~93.9%,相对标准偏差均<10%。应用该方法对76份鸡蛋样品进行检测,共检出阳性样品7份,检出率为9.21%。结论该方法简便、准确,适用于鸡蛋中喹诺酮类和四环素类药物残留量的同时检测。
Objective To establish a method for the determination of 11 quinolines and 10 tetracycline residues in eggs by ultra high performance liquid chromatography coupled with electrospray tandem mass spectrometry（UPLC-MS/MS）.Methods The target antibiotics in samples were extracted ultrasonically with EDTA-Mcllvaaine solution.After filtration and centrifugation,the supernatant was cleaned up with HLB column.The sample solution was separated on an acquity BEH C18column（2.1 mm ×100 mm,1.7 μm） with gradient elution using acetronitrile-0.2% formic acid as mobile phase.Identification was performed with tandem mass spectrometer,with electrospray ionization（ESI） in positive mode under multiple reaction monitoring.The quantification was based on external standard curves.Results The method showed good linearity in the range of 2 μg/kg-100 μg/kg（r 〉0.994 0）.The detection limits of the method were within 0.5 μg/kg-2.0 μg/kg.The recoveries ranged from79.5% to 93.9%,and the relative standard deviations were all less than 10%.Quinoline and tetracycline residues were detected in 9.21% of 76 egg samples which were determined by this method.Conclusion The method is rapid,specific,accurate and it is suitable for the detection of quinolone and tetracycline residues.
作者
王敏娟
胡佳薇
田丽
乔海鸥
聂晓玲
WANG Min-juan HU Jia-wei TIAN Li QIAO Hai-ou NIE Xiao-ling(Physical and Chemical Laboratory, Shanxi Provincical Center for Disease Control and Prevention, Xi＇an, Shaanxi 710054, China)
出处
《中国卫生检验杂志》
CAS
2017年第4期473-476,共4页
Chinese Journal of Health Laboratory Technology
关键词
液相色谱-质谱
喹诺酮
四环素
鸡蛋
Liquid chromatography mass spectrometry
Quinolone
Tetracycline
Egg
