色谱

色谱 ›› 2017, Vol. 35 ›› Issue (7): 677-682.DOI: 10.3724/SP.J.1123.2017.03009

• 研究快报 • 上一篇    下一篇

超高效液相色谱-串联质谱法快速测定牛奶中螺虫乙酯及其代谢物残留

易廷辉1, 唐柏彬2, 邹芸3, 郗存显2, 王国民2   

  1. 1. 重庆市农业生态与资源保护站, 重庆 401121;
    2. 重庆出入境检验检疫局, 重庆市进出口食品安全工程技术研究中心 重庆 400020;
    3. 重庆市市政环卫监测中心, 重庆 401121
  • 收稿日期:2017-03-08 出版日期:2017-07-08 发布日期:2013-10-18
  • 通讯作者: 王国民,Tel:(023)67733645,E-mail:chqwgm@163.com
  • 基金资助:

    国家认监委出入境检验检疫行业标准项目（2014B086）.

Rapid determination of spirotetramat and its metabolite residues in milk by ultra performance liquid chromatography-tandem mass spectrometry

YI Tinghui1, TANG Bobin2, ZOU Yun3, XI Cunxian2, WANG Guomin2   

  1. 1. Chongqing Agricultural Ecological Environment & Resources Protection Station, Chongqing 401121, China;
    2. Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing 400020, China;
    3. Chongqing Municipal & Environmental Sanitation Monitoring Department, Chongqing 401121, China
  • Received:2017-03-08 Online:2017-07-08 Published:2013-10-18
  • Supported by:

    Entry-Exit Inspection and Quarantine Trade Standard Item of Certification and Accreditation Administration (No.2014B086).

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121

被引次数

6

摘要：

建立了超高效液相色谱-串联质谱快速测定牛奶中螺虫乙酯及其代谢物残留的分析方法。牛奶经乙腈沉淀蛋白质，正己烷脱脂后，采用ESI源，在MRM模式下测定螺虫乙酯及其代谢物。结果表明，在0.5~50 μ g/L范围内，待测物色谱峰面积与其质量浓度间的线性关系良好（相关系数均大于0.998），检出限（LODs，S/N=3）和定量限（LOQs，S/N=10）分别为0.05~0.30 μ g/L和0.17~1.00 μ g/L。当添加水平为1.0、2.0和10 μ g/L时，方法的加标回收率为80.0%~108.8%，相对标准偏差（RSD）为4.8%~15.2%（n=6）。该法快速，灵敏，准确，能够满足牛奶中螺虫乙酯及其代谢物残留限量的检测要求。

关键词: 超高效液相色谱-串联质谱, 代谢物, 螺虫乙酯, 牛奶

Abstract:

A method for the rapid and simultaneous determination of spirotetramat (BYI08330) and its four metabolites in milk was developed with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with acetonitrile for precipitating proteins, degreased with hexane, and analyzed by UPLC-MS/MS in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Good linear relationships between peak areas and mass concentrations of the analytes were obtained in the range of 0.5-50 μ g/L with correlation coefficients greater than 0.998 (n=6). The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were 0.05-0.30 μ g/L and 0.17-1.00 μ g/L, respectively. The recoveries at the spiked levels of 1.0, 2.0 and 10 μ g/L were in the range of 80.0%-108.8% with relative standard deviations (RSDs) of 4.8%-15.2% (n=6). The method is fast, sensitive and accurate, and can be used to simultaneously determine BYI08330 and its four metabolites in milk.

Key words: metabolites, milk, spirotetramat (BYI08330), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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