用超高效液相色谱-串联质谱法同时检测浓缩饲料中的多种兽药残留  

Determination of Multi-veterinary Drugs in the Concentrated Feed by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘瑜[1] 赵颖[1] 李晓东[1] 金雁[1] 蒋施[1] 徐宜宏[1] 钟钰[1] 曾凡[1] 于丽[1] 周健南[1] 

机构地区：[1]沈阳出入境检验检疫局,辽宁110016

出　　处：《化学通报》2013年第2期157-162,共6页Chemistry

基　　金：辽宁出入境检验检疫局科技项目(LK21-2009)资助

摘　　要：建立了浓缩饲料中6种喹诺酮类兽药、14种磺胺类兽药、3种硝基呋喃类兽药、6种大环内酯类兽药共29种兽药残留检测的超高效液相色谱-串联质谱分析方法。样品经甲醇-乙腈(体积比1∶1)混合溶液提取,提取液经Oasis HLB固相萃取柱净化,29种兽药经Waters Acquity UPLC BEH C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱。电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,内标法定量。结果表明,29种兽药在0.01～5.0mg/mL范围内呈良好的线性关系,相关系数(r)均大于0.993;浓缩饲料中3个浓度添加水平平均回收率为61.4%～93.3%;相对标准偏差为2.62%～13.9%。An ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） method was established for the determination of 29 veterinary drugs residues in which including 6 quinolones, 14 sulfonamides,3 nitrofurans and 6 macrolides, in the concentrated feed. Samples were extracted with methanol-aeetonitrile （1：1） solution. Extraction liquid was purified by Oasis HLB SPE column. The separation of 29 veterinary drugs was performed on a Waters Aequity UPLC system with a BEH Cls column. The mobile phases were acetonitrile and water （containing 0.1% formic acid）in gradient elution. The electrospray was operated in the positive ionization mode and the 29 veterinary drugs were identified by multiple reaction monitoring（MRM） mode. Internal standard method was adopted as the quantitative method. The calibration curves showed good linearity within the concentrations of 0. 01 - 5.0mg/mL with the correlation coefficients r 〉 0. 993. The recoveries of 29 veterinary drugs were 61.4% -93.3% at three spiked levels. The relative standard deviations were 2. 62% - 13.9%.

关 键 词：超高效液相色谱-串联质谱 兽药 浓缩饲料 

分 类 号：S816[农业科学—饲料科学]