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作 者:易可可 谢洁 江游[2] 乔晓婷 龚晓云[2] 黄泽建[2] 翟睿 彭涛 戴新华[2] 方向[2] 时国庆[1] YI Ke-Ke;XIE Jie;JIANG You;QIAO Xiao-Ting;GONG Xiao-Yun;HUANG Ze-Jian;ZHAI Rui;PENG Tao;DAI Xin-Hua;FANG Xiang;SHI Guo-Qing(Faculty of Chemical and Biological Engineering University of Science and Technology Beijing,Beijing 100083,China;Center for Mass Spectrometry Engineering Technology,China Metering Frontiers Science Center Research Institute,Beijing 100029,China)
机构地区:[1]北京科技大学化学与生物工程学院,北京100083 [2]中国计量科学研究院前沿计量科学中心,质谱仪器工程技术研究中心,北京100029
出 处:《食品安全质量检测学报》2020年第16期5562-5568,共7页Journal of Food Safety and Quality
基 金:国家重点研发计划项目(2019YFF0216303、2016YFF0200502、2016YFF0200504)。
摘 要:目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)同时测定猪肉中3种β-受体激动剂类药物(沙丁胺醇、莱克多巴胺、克伦特罗)的检测方法。方法制备的样品用含1%乙酸的乙腈提取,正己烷去脂后,采用ZORBAX SB-C18色谱分离,采用乙腈-0.1%甲酸(含5 mmol/L乙酸铵)梯度洗脱,多反应监测模式定量。结果本方法在12 min内完成3种目标化合物的分离分析。方法的检出限为0.003~0.015μg/kg,定量限为0.01~0.05μg/kg。在0.01~5μg/kg的添加范围内,动物肌肉组织中添加回收率为71.6%~112.6%,相对标准偏差为7.2%~16.9%。结论该方法快速、准确、灵敏,适合同时定量猪肉中3种β-受体激动剂类药物残留测定。Objective To establish a method for the simultaneous quantification of 3 kinds of β-agonist stimulant drugs(salbutemol, ractopamine, clenbuterol) in pork by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods The prepared samples were extracted with acetonitrile containing 1% acetic acid and acetonitrile saturated n-hexane, and then separated by ZORBAX SB-C18 chromatography. The mobile phase was acetonitrile-0.1% formic acid, with a gradient elution, and the content of β-agonist stimulant drugs was quantified by multiple reaction monitoring(MRM) mode. Results This method completed the analysis of 3 target compounds within 12 min. The limits of detection were 0.003–0.015 μg/kg, and the limits of quantitation were 0.01–0.05 μg/kg. Average recoveries were found in the range of 71.6%–112.6% at the addition to animal muscle tissue of 0.01–5 μg/kg with relative standard deviations of 7.2%–16.9%. Conclusion This method is rapid, accurate and sensitive, and suitable for simultaneous determination of 3 β-agonist drugs residues in pork.
关 键 词:动物源性食品 液相色谱-串联质谱法 禁用兽药
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