色谱

色谱

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高效液相色谱-串联质谱法测定食品中多杀菌素A和D的残留量

张缙, 杨黎忠, 林立毅, 陈鹭平, 周昱, 徐敦明*   

  1. 厦门出入境检验检疫局检验检疫技术中心, 福建 厦门 361026
  • 收稿日期:2011-03-18 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 徐敦明,博士,高级工程师,研究方向为食品安全. Tel: (0592)3269935,
  • 基金资助:

    厦门市科技计划项目(3502Z20092009、3502Z20102012)和国家质检总局科技计划项目(2010IK192)

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

ZHANG Jin, YANG Lizhong, LIN Liyi, CHEN Luping, ZHOU Yu, XU Dunming*   

  1. Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China
  • Received:2011-03-18 Online:2011-07-28 Published:2011-08-19

PDF

353

被引次数

33

摘要： 建立了食品中多杀菌素(spinosyn) A和D残留的液相色谱-串联质谱(HPLC-MS/MS)检测方法。甘蓝等食品样品经乙腈-水(50:50, v/v)提取、HLB固相萃取柱净化后,采用HPLC-MS/MS进行检测分析,利用外标法定量。质谱分析采用电喷雾电离,正离子扫描,多反应监测模式。结果表明,柱净化后无明显的基质效应,多杀菌素在1～20 μg/L内具有较好的线性关系,其相关系数可达0.9999;样品中添加1～10 μg/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%;检出限(信噪比（S/N）=3): 多杀菌素A为0.2 μg/kg,多杀菌素D为0.5 μg/kg;定量限(S/N=10): 多杀菌素A为0.5 μg/kg,多杀菌素D为1.0 μg/kg。在最佳实验条件下,对来自福建厦门的969份食品样品进行了检测,其中15份样品检测结果呈阳性。实验结果表明,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: 多杀菌素, 多杀菌素A, 多杀菌素D, 高效液相色谱-串联质谱法, 食品

Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of spinosyns A and D residues in foodstuffs. The food samples were extracted with acetonitrile-water (50:50, v/v), and then purified by an HLB solid phase extraction (SPE) column. The analytes were determined by HPLC-MS/MS and quantified by external standard method. The mass spectrometric detection was operated with electrospray in positive ionization mode and the spinosyns A and D were identified in multiple reaction monitoring (MRM) mode. The linear range of the method was 1-20 μg/L, with the correlation coefficient (r2) of 0.9999. No significant matrix effect was found for spiked samples. The recoveries of spinosyns A and D spiked in food were 76.2%-114.0% at the spiked levels of 1-10 μg/kg. The relative standard deviations (RSDs) were less than 10%. The limits of detection (LODs) and quantification (LOQs) were 0.2 μg/kg and 0.5 μg/kg for spinosyn A, 0.5 μg/kg and 1.0 μg/kg for spinosyn D, respectively. The proposed procedure was applied to the analysis of 969 real samples from Xiamen, Fujian Province (China), of which 15 positive samples were found. The results showed that the proposed method is sensitive and accurate for the determination of spinosyns A and D in foodstuffs.

Key words: food, spinosyn D, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), spinosad, spinosyn A