摘要
目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定禽蛋类中4种四环素类(tetracyclines,TCs)抗生素残留量的分析方法。方法样品经含50μg/mL蛋白酶K—0.1 mol/L EDTA-Na2溶液提取, Prime HLB固相萃取小柱净化,洗脱液用氮气吹至近干,用含甲醇和0.1%甲酸水(4+6)溶液溶解,采用多反应监测正离子模式,定性和定量测定禽蛋类中的四环素、土霉素、金霉素、强力霉素等4种四环素类抗生素。结果 4种四环素类抗生素在5～200μg/L范围内呈现良好的线性关系,相关系数均大于0.999;方法的检出限为0.3μg/kg,定量限为1.0μg/kg;添加水平为20.0～200μg/kg时,平均回收率为80.5%～124%,相对标准偏差(relative standard deviation,RSD)为0.89%～6.8%。结论该方法简单、快捷,可作为禽蛋类中四环素类抗生素的检测方法。
Objective To establish a method for the determination of 4 tetracycline(TCs) kinds of antibiotics residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by the solution including 50 μg/mL proteinase K and 0.1 mol/L EDTA-Na 2 , and the extracts were cleaned-up on Prime HLB solid phase extraction column, and the eluent which got from above conditions was dried nearly by nitrogen-blow, and dissolved in methanol and 0.1% formic acid (4+6). Finally, the qualitative and quantitative determination of the target analytes were detected by UPLC-MS/MS in multiple reaction monitoring(MRM)mode. Results The results showed that 4 kinds of tetracyclines had good linear relationships in the range of 5-200 μg/L with correlation coefficients better than 0.999. The limits of detection were 0.3 μg/kg and the limits of quantitation were 1.0 μg/kg. The average recoveries of the method ranged from 80.5% to 124% at the spiked levels of 20.0-200 μg/kg for the 4 kinds of TCs, with the relative standard deviations (RSD) of 0.89%-6.8%. Conclusion This method is simple and quick, which can be used as the detection method of antibiotic residues in
作者
薛荣旋
刘国平
黄诚
丘福保
林胜军
XUE Rong-Xuan;LIU Guo-Ping;HUANG Cheng;QIU Fu-Bao;LIN Sheng-Jun(Zhongshan Center for Disease Control and Prevention, Zhongshan 528400, China)
出处
《食品安全质量检测学报》
CAS
2018年第23期6247-6252,共6页
Journal of Food Safety and Quality
关键词
蛋白酶K
超高效液相色谱-串联质谱法
四环素类抗生素
禽蛋类
proteinase K
ultra performance liquid chromatography-tandem mass spectrometry
tetracycline antibiotics
egg
