摘要
建立一种超高效液相色谱串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)快速测定禽蛋中恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星、洛美沙星和沙拉沙星共7种喹诺酮类兽药残留的分析方法.禽蛋样品经体积分数为5%的甲酸-乙腈提取喹诺酮类兽药残留,QuEChERS净化后通过快速溶剂蒸发系统浓缩,采用C18色谱柱分离,以体积分数为0.1%的甲酸和乙腈为流动相进行梯度洗脱,电喷雾离子源电离,多反应监测模式采集信号,基质外标法定量.结果表明,7种喹诺酮类兽药在2.0~100.0 ng/mL线性关系良好(R^2>0.995),方法的检出限和定量限分别为0.3和1.0μg/kg;添加2、5、10μg/kg三个浓度水平,平均回收率为77.20%~98.47%,相对标准偏差为1.5%~6.2%(n=6).该方法简单快捷、准确度好、灵敏度高,适用于禽蛋中喹诺酮类兽药残留的快速确证.
An analytical method for rapid determination of enrofloxacin,ciprofloxacin,ofloxacin,pefloxacin,norfloxacin,lomefloxacin and sarafloxacin in poultry eggs by QuEChERS and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The quinolone residues in poultry eggs were extracted by 5%( V/V ) formic acid-acetonitrile mixed solution,purified by QuEChERS and concentrated by a rapid solvent evaporation system,and separated on a C 18 column with a mobile phase consisted of 0.1%( V/V ) formic acid solution and acetonitrile by gradient elution. The quinolone residues were determined in a multiple reaction monitoring (MRM) mode by the electrospray ionization source (ESI^+) and quantified with a matrix external standard method. The results showed that all the seven quinolones had good linearity in the concentration range of 2.0-100.0 ng/mL with the correlation coefficients greater than 0.995. The limits of detection (LOD) and limits of quantitation (LOQ) of the method were 0.3 μg/kg and 1.0 μg/kg,respectively,the average recovery rate was 77.20%-98.47%,and the relative standard deviation was 1.5%-6.2%. This method is easy,accurate and sensitive,which is suitable for rapid detection of quinolone residues in poultry eggs.
作者
黄坤
范小龙
曹琦
韩智
张莉
王会霞
郭嘉
HUANG Kun;FAN Xiaolong;CAO Qi;HAN Zhi;ZHANG Li;WANG Huixia;GUO Jia(Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075,China;Key Laboratory for Green Chemical Process of Ministry of Education, School of Chemical Engineering and Pharmacy,Wuhan Institute of Technology,Wuhan 430205,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2019年第16期261-265,共5页
Food and Fermentation Industries
基金
“十三五”国家重点研发计划重点专项(2018YFC1604 000)
