摘要
建立了蔬菜中二氟沙星、达氟沙星、沙拉沙星、氧氟沙星、恩诺沙星、培氟沙星、环丙沙星、诺氟沙星等8种喹诺酮类抗生素残留的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。蔬菜中喹诺酮类抗生素残留经酸化乙腈提取、N-丙基乙二胺(PSA)和石墨化炭黑(GCB)吸附剂净化后用于HPLC-MS/MS检测,以乙腈和水(0. 1%甲酸)为流动相,经C18(2. 1×150 mm,3. 5μm)色谱柱分离后,在正离子模式下采用多反应监测模式进行测定。蔬菜中8种喹诺酮类抗生素残留分析方法的线性范围为5~200μg/kg,检出限为1μg/kg,在10,50,100μg/kg 3个浓度水平下进行加标回收实验,平均回收率为71. 5%~111%,相对标准偏差为1. 3%~10%。该方法适用于蔬菜中喹诺酮类抗生素残留的快速分析。
A high performance liquid chromatography-electrospray ionization triple-quadruple tandem mass spectrometric method was established for the determination of quinolones,including difloxacin,danofloxacin,sarafloxacin,ofloxacin,enrofloxacin,pefloxacin,ciprofloxacin and norfloxacin in vegetables.The 8 target quinolones in vegetables were extracted with acidified acetonitrile,and then purified with primary secondary amine(PSA)and GCB sorbent.The reconstituted sample solution was analyzed by HPLC-MS/MS under positive ion mode,with C18 column(2.1×150 mm,3.5μm)as the analytical column.The detection limits of all the 8 quinolones were 1μg/kg with the linear range from 5μg/kg to 200μg/kg.The recovery of the method was validated at 10,20 and 50μg/kg,respectively,and the average recoveries were in the range of 71.5%-111%,with the relative standard deviations between 1.3%and 10%.With the advantages of simplicity and high sensitivity,the method is suitable for the determination of quinolones in vegetables.
作者
王晓利
郭涛
苑金鹏
王珊珊
李磊
赵汝松
WANG Xiao-li;GUO Tao;YUAN Jin-peng;WANG Shan-shan;LI Lei;ZHAO Ru-song(Analysis and Test Center,Qilu University of Technology(Shandong Academy of Sciences),Jinan 250014;Shandong Academy of Agricultural Sciences,Shandong Rice Research Institute,Jinan 250010)
出处
《分析试验室》
CAS
CSCD
北大核心
2019年第8期916-920,共5页
Chinese Journal of Analysis Laboratory
基金
山东省重点研发计划项目(2018GSF117036)资助
