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液相色谱-串联质谱法测定食品中多杀菌素A和D 残留量

张缙1,杨黎忠1,林立毅2,陈鹭平2,周昱1,徐敦明1   

  1. 1. 厦门出入境检验检疫局检验检疫技术中心
    2.
  • 收稿日期:2011-03-18 修回日期:2011-05-20 出版日期:2011-05-23 发布日期:2011-05-23
  • 通讯作者: 徐敦明

Determination of spinosyn A and D residues in food by high performance liquid chromatography—tandem mass spectrometry

  • Received:2011-03-18 Revised:2011-05-20 Online:2011-05-23 Published:2011-05-23
  • Contact: Dun-Ming Xu

摘要： 建立了食品基质中多杀菌素（spinosyn）A和D残留的液相串联质谱检测方法。柚子等样品经乙腈-水（50：50，v/v）提取，经HLB柱净化，采用液相色谱串联质谱分析，外标法进行定量。质谱分析采用电喷雾电离，正离子扫描，多反应监测模式。对多杀菌素主要碎片的裂解方式进行了剖析。实验证明，柱净化后无明显的基质效应，样品中添加1～10μg/kg的多杀菌素，其回收率为76.2 ％ ～114.0％，相对标准偏差(n=10)小于10％ ；多杀菌素A检出限为0.2μg/kg，定量限为0.5μg/kg；多杀菌素D检出限为0.5μg/kg，定量限为1.0μg/kg。该方法提取效果好，具有良好的灵敏度、回收率和重复性。

关键词: 残留, 多杀菌素, 食品, 液相串联质谱法

Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of spinosyn A and D in foodstuffs．The residues in food were extracted with acetonitrile-water(50:50, v/v)，and purified by a HLB SPE column. The mass spectrometry was operated with electrospray in positive ionization mode and spinosyn A and D were identified in multiple reaction monitoring (MRM)mode. The fragmentation pathways for the main product ions were analyzed．No significant matrix effect was found for spiked samples．The recoveries of spinosyn A and D spiked in food were 76.2%-114.0% at spiked levels of 1-10μg/kg．The relative standard deviations (RSDs) were less than 10%．The limits of quantitation (LOQs) were 0.5μg/kg for spinosyn A, 1.0μg/kg for spinosyn D．This method is sensitive and accurate in the determination of spinosyn A and D in foodstuffs．

Key words: (HPLC-MS/MS), food, residue, spinosyn A and D

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