多壁碳纳米管分散固相萃取结合LC-MS/MS测定饲料中11种β-受体激动剂  

Analysis on 11 β-recptor Agonists in Feeds by LC-MS/MS Coupled with Dispersive Solid Phase Extraction Using Multiwalled Carbon Nanotubes as Absorbent

作　　者：应永飞[1,2] 朱聪英[2] 陈慧华[2] 韦敏珏[2] 周炜[2] 汪以真[1] 

机构地区：[1]浙江大学动物科学学院,浙江杭州310058 [2]浙江省畜产品质量安全检测中心,浙江杭州310020

出　　处：《中国畜牧杂志》2013年第9期68-73,共6页Chinese Journal of Animal Science

基　　金：公益性行业(农业)科研专项(201203023-4);浙江省重点科技创新团队(2010R50028)

摘　　要：本研究建立了采用多壁碳纳米管(MWCNTs)为吸附剂的分散固相萃取(dSPE)净化、液相色谱串联质谱测定饲料中11种β-受体激动剂(克伦特罗、莱克多巴胺、沙丁胺醇、苯乙醇胺A、氯丙那林、妥布特罗、西马特罗、特布他林、马布特罗、班布特罗和喷布特罗)的方法。饲料样品经甲酸水溶液提取后,调节pH值至10,加入50 mgMWCNTs进行分散固相萃取,被吸附的化合物经1.0%甲酸水甲醇(91)洗脱,洗脱液过滤膜后进行LC-MS/MS分析。采用Acquity UPLC BEH C18色谱柱分离,以0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱,电喷雾正电子(ESI+)模式电离,多反应监测(MRM)模式监测,内标法校准进行定量。结果表明:11种β-受体激动剂在0.1～20μg/L浓度范围内呈良好的线性,线性相关系数均大于0.997,猪配合饲料样品中最低定量限为0.05～0.48μg/kg。猪配合饲料中添加0.5～500μg/kgβ-受体激动剂的回收率在89.6%～112.9%,相对标准偏差RSD均小于15%。A simple, sensitive and reliable analytical method was developed for 13-recptor agonists （clenbuterol, ractopamine, salbutamol, pheny/ethanolamine A, clorprenaline, tulobuterol, cimaterol, terbutaline, mahuterol, bambuterol, penbuterol） in feeds by ultra high performance liquid chromatography-positive electrospray ionisation tandem mass spectrometry （UHPLC-ESI-MS/MS） using dispersive solid phase extraction （dSPE） with multi-walled carbon nanotubes （MWCNTs）. Feed samples were extracted using formic acid solution. After adjusting pH value to 10, 50 mg of MWCNTs were added to absorpt [3-recptor agonists and 1.0 % formic acid solution： methanol （9：1 v/v） was used to elute the compounds from the MWCNTs. The eluate was directly analyzed by LC-MS/MS on an Acquity UPLC BEH C^s column with a mixture of methanol and 0.1% formic acid solution as the mobile phase. The samples were quantified with the internal standard calibration curve method. Good linearities were obtained for the β-recptor agonists at the concentration of 0.1-20 /.zg/L with the linear relative coefficient more than 0.997. The recoveries for the β2-agonists in mixed feeds were 89.6%-112.9% at the fortified levels of 0.5-500/zg/kg with the limit of quantitation of 0.05μg/kg -0.48μg/L. The relative standard deviations were less than 15.0%.

关 键 词：β-受体激动剂 多壁碳纳米管 分散固相萃取 液相色谱串联质谱法 

分 类 号：S816.730.17[农业科学—饲料科学]