超高效液相色谱-串联质谱测定牛奶中喹赛多残留  

Determination of cyadox in milk by UPLC-MS/MS

作　　者：马晓年[1] 张秀清[1] 陈俊秀[1] 欧利华[1] MA Xiao-nian;ZHANG Xiu-qing;CHEN Jun-xiu;OU Li-hua(Kunming Center for Disease Control and Prevention,Kunming 650228,China)

机构地区：[1]昆明市疾病预防控制中心,昆明650228

出　　处：《湖北农业科学》2020年第21期144-146,共3页Hubei Agricultural Sciences

基　　金：昆明市卫生人才科技人才培养项目[2017-sw(后备)-66;2019-sw(后备)-50]。

摘　　要：采用超高效液相色谱-串联质谱法检测牛奶中喹赛多,样品经乙酸乙酯提取,经PEP固相萃取柱净化、富集,以乙腈/甲醇(3∶11)-0.1%甲酸水为流动相,经岛津Inertsil ODS-3柱(3μm,2.1 mm×100 mm)色谱柱分离,采用多反应检测正离子模式进行定性及定量分析。结果表明,PEP固相萃取柱具有较好的回收率,喹赛多的检出限为0.01μg/g,定量限为0.04μg/g,在0.384、0.960、1.920μg 3个加标水平下回收率分别为136.0%、116.0%、62.6%。该法灵敏度高、重复性好,可满足牛奶样品中喹赛多残留的测定。To establish a reliable pretreatment method for cyadox in milk with UPLC-MS/MS.The sample was extracted by ethyl acetate,then the results was analysed after PEP cartridge purification.The objective compounds were separated using Inertsil ODS-3column(3μm,2.1 mm×100 mm)with acetonitrile/methanol(3∶11)-water(0.1%formate)as mobile phase and analyzed by mass spectrometry in the positive electrospray ionization under multiple reaction monitoring mode(MRM).The results showed that PEP cartridge had good recovery rate.The detection limit of cyadox was 0.01μg/g,limit of quantitation was 0.04μg/g,the average recoveries for spiked levels of 0.384,0.960,1.920μg were 136.0%,116.0%,62.6%.The method is suitable for the detection of cyadox residual in milk.

关 键 词：喹赛多 固相萃取小柱 超高效液相色谱-串联质谱 牛奶 

分 类 号：O657.7[理学—分析化学] S859.84[理学—化学]