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| 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 | |
| 引用本文： | 应永飞,朱聪英,陈慧华,韦敏珏,周炜,汪以真.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[J].中国畜牧杂志,2013,49(9). |
| 作者姓名： | 应永飞 朱聪英 陈慧华 韦敏珏 周炜 汪以真 |
| 作者单位： | 1. 浙江大学动物科学学院,浙江杭州310058;浙江省畜产品质量安全检测中心,浙江杭州310020 2. 浙江省畜产品质量安全检测中心,浙江杭州,310020 3. 浙江大学动物科学学院,浙江杭州,310058 |
| 基金项目： | 公益性行业(农业)科研专项，浙江省重点科技创新团队 |
| 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(91)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%。 |
| 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 |
Analysis on 11 β-recptor Agonists in Feeds by LC-MS/MS Coupled with Dispersive Solid Phase Extraction Using Multiwalled Carbon Nanotubes as Absorbent |
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| YING Yong-Fei , ZHU Cong-Ying , CHEN Hui-Hua , WEI Min-Jue , ZHOU Wei , WANG Yi-Zhen.Analysis on 11 β-recptor Agonists in Feeds by LC-MS/MS Coupled with Dispersive Solid Phase Extraction Using Multiwalled Carbon Nanotubes as Absorbent[J].Chinese Journal of Animal Science,2013,49(9). | |
| Authors: | YING Yong-Fei ZHU Cong-Ying CHEN Hui-Hua WEI Min-Jue ZHOU Wei WANG Yi-Zhen |
| Abstract: | A simple,sensitive and reliable analytical method was developed for β-recptor agonists(clenbuterol,ractopamine,salbutamol,phenylethanolamine A,clorprenaline,tulobuterol,cimaterol,terbutaline,mabuterol,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 β-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 C18 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 μg/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 μg/kg with the limit of quantitation of 0.05 μg/kg ~0.48 μg/L.The relative standard deviations were less than 15.0%. |
| Keywords: | β-recptor agonists MWCNTs dispersive solid phase extraction liquid chromatography with tandem mass spectrometry |
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