液相色谱-四极杆-飞行时间质谱法对常见兽药残留同时检测的方法探究  

The Study on Screening Method by LC-Q-TOF for Veterinary Drug Residues Analysis

作　　者：王珮[1,2] 汤志旭[2] 国彤彤 高昕[1] 

机构地区：[1]中国海洋大学食品科学与工程学院,山东青岛266003 [2]山东出入境检验检疫局,山东青岛266001

出　　处：《农产品加工（下）》2015年第3期46-50,57,共6页Farm Products Processing

基　　金：国家质检总局科技计划项目(2013IK039)

摘　　要：利用液相色谱-四极杆-飞行时间质谱技术,对7类45种兽药残留同时检测方法进行探究。经BAP-SPE固相萃取柱富集净化,甲醇、1%甲酸乙腈和10%甲醇乙酸乙酯依次洗脱,吹干后纯水-乙腈（V/V,9∶1）定容上机检测。45种目标物经Agilent Extend C18型色谱柱分离,分别以含0.1%甲酸的5 m M乙酸铵-乙腈为流动相进行ESI＋正离子采集和5 m M乙酸铵-乙腈为流动相进行ESI-负离子采集。结果显示,7类45种兽药在1~500μg/L时线性关系良好,相关系数均大于0.99,仪器测定低限LOD在0.50~20.00μg/L,方法检出限均在0.25μg/L以下。除磺胺胍回收率为58.85%外,其余目标物回收率均在70.22%~120.69%,相对标准偏差RSD为1.18%~22.03%。该方法灵敏度高、准确性好,满足兽药多残留的筛查检测要求。This paper aim at exploring a method for 7 kinds of 45 veterinary drug residues detection by using liquid chromatography-quadrupole-time-of-flight（LC-Q-TOF） tandem mass spectrometry. By using BAP-SPE solid phase to extract and purity,Me OH,Acetonitrile containing 1.0%（V/V） formic acid and Ethyl Acetate containing 10%（V/V） Me OH to elute successively,vaporat by a streamof nitrogen then add purity water-ACN（V/V,9∶1） to be ready for injection. The45 target compounds are separated by Agilent Extend C18 column with the gradient elution using two mobile phases and two different acquisition modes seperately：acetonitrile and 5 m M ammonium acetate mobile phase containing 0.1% formic acid with ESI＋ mode,and acetonitrile and 5 m M ammonium acetate mobile phase with ESI- mode. The results show that the7 kinds of 45 veterinary drugs had good relationshiop in range of 1~500 μg/L,the linear correlation coefficient are greater than0.99,LOD of instrument is 0.50~20.00 μg/L,LOD of method is lower than 0.25 μg/L. Despite SGD recovery rate is 58.85%,all rest recovery rates are 70.22% ~120.69%, the relative standard deviation are 1.18% ~22.03%. This method has high sensitivity and good accuracy,which can be used to screen the multi-veterinary residues.

关 键 词：液相色谱-四极杆-飞行时间质谱(LC-Q-TOF) 兽药多残留 同时检测 

分 类 号：O658[理学—分析化学]