液相色谱-串联质谱法同时测定猪肉中3种β-受体激动剂的残留量

Simultaneous determination of 3 kinds of β-agonist residues in pork by liquid chromatography-tandem mass spectrometry

中文关键词:  动物源性食品  液相色谱-串联质谱法  禁用兽药

英文关键词:animal derived food  liquid chromatography-tandem mass spectrometry  banned veterinary drugs

中文摘要:

      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0.003~0.015 μg/kg, 定量限为0.01~0.05 μg/kg。在0.01~5 μg/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。

英文摘要:

      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.