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超高效液相色谱-四极杆-飞行时间质谱法快速筛查动物组织中7种β-受体激动剂残留

Rapid Screening of β-Agonists Residues in Animal Tissue by Ultra High Performance Liquid Chromatography Coupled with Quadrupole-Time of Flight Mass Spectrometry

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【作者】 蒋万枫赵珊

【Author】 JIANG Wan-feng,ZHAO Shan*(Qingdao Quality Supervision and Inspection Center for Shopping Basket Commodity,Qingdao 266071,China)

【机构】 青岛市菜篮子商品质量监督检测中心

【摘要】 建立了超高效液相色谱-四极杆-飞行时间质谱法(UHPLC-Q-TOF-MS)快速筛查动物组织中7种β-受体激动剂残留(特布他林、沙丁胺醇、塞布特罗、莱克多巴胺、克伦特罗、溴布特罗、马布特罗)的检测方法。样品经乙酸铵提取,固相萃取净化后,进行UHPLC-Q-TOF-MS测定。根据分析软件,通过理论精确相对分子质量与所测得的精确相对分子质量之间匹配度,以及目标化合物的元素组成分析,结合保留时间、同位素丰度模型和子离子特征,对目标化合物进行确证。结果表明:7种β-受体激动剂在4个加标水平的加标回收率为75%~114%,RSD为4.5%~20.6%。该方法的相关系数(r2)为0.991 4~0.999 9,除克伦特罗的线性范围为0.4~40.0μg/kg,定量下限为0.4μg/kg外,其余化合物的线性范围均为0.2~40.0μg/kg,定量下限为0.2μg/kg。

【Abstract】 An analytical method was established for the determination of β-agonists(e.g.terbutaline,salbutamol,cimbuterol,ractopamine,clenbuterol,brombuterol,mabuterol)residues in animal tissue by ultra high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UHPLC-Q-TOF-MS).The samples were extracted with ammonium acetate,and determined by UHPLC-Q-TOF-MS after solid phase extraction.By software,the targeted compound was confirmed by the diff between theoretical accurate relative molecular mass(Mr) and the actual accurate Mr,element composition analysis,retention time,isotopic abundance model and product ion characteristics.The result indicated that the average recoveries were in the range of 75%-114% with relative standard deviations of 4.5%-20.6%.The calibration curves were linear in the ranges of 0.4-40.0 μg/kg for clenbuterol,and 0.2-40.0 μg/kg for the rest of the compounds,with correlation coefficients of 0.991 4-0.999 9.The limits of quantitation were 0.4 μg/kg for clenbuterol and 0.2 μg/kg for the other compounds.

【基金】 青岛市“菜篮子”专项资金(青财企[2011]77号)
  • 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2013年06期
  • 【分类号】O657.63;TS251.7
  • 【被引频次】18
  • 【下载频次】171
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