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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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