摘要
建立了复合预混饲料中29种兽药同时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(1:1,V/V)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,以甲醇和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,多反应监测模式检测,内标法定量。结果表明:29种兽药在0.01～5.0μg/mL范围内呈良好的线性关系,相关系数(r)均大于0.993;复合预混饲料中3个浓度添加水平平均回收率为65.5%～92.2%;相对标准偏差为3.8%～15%。
An ultra performance liquid chromatography-tandem mass spectrometric （UPLC-MS/MS）method was established for the determination of 29 veterinary drug. （6 quinolone drugs, 14 sulfonamide drugs, 3 nitrofuran drugs,6 macrolide drugs ）residues in the compound premix feed. Samples were extracted with methanol- acetonitrile（50：50, V/V）solution. Extraction liquid was purified by an Oasis HLB SPE column. The separation of 29 veterinary drugs was performed on a Waters Acquity UPLC system with a BEH Cls column. The mobile phase was methanol 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 - 5.0 μg/mL with the correlation coefficients r 〉 0. 993. The recoveries of 29 veterinary drugs were 65.5% -92. 2% were both less than 3.8% - 15%. This method is simple at three spiked levels. The relative standard deviations , sensitive and accurate in the determination of veterinary drug residues.
出处
《分析试验室》
CAS
CSCD
北大核心
2012年第10期77-81,共5页
Chinese Journal of Analysis Laboratory
基金
辽宁出入境检验检疫局科技项目(LK21-2009)资助
关键词
超高效液相色谱-串联质谱
兽药
复合预混饲料
Ultra performance liquid chromatography-tandem mass spectrometry
Veterinary drug
Compound premix feed
作者简介
刘瑜(1982-),女,工程师,E-mail:liuyu-0117@163.com
