色谱

色谱 ›› 2018, Vol. 36 ›› Issue (8): 752-757.DOI: 10.3724/SP.J.1123.2018.03014

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱法同时测定牛奶和羊奶中莫奈太尔及其代谢产物残留

吴映璇, 谢敏玲, 姚仰勋, 蓝草   

  1. 广东检验检疫技术中心, 广东省动植物与食品进出口技术措施研究重点实验室, 广东 广州 510623
  • 收稿日期:2018-03-15 出版日期:2018-08-08 发布日期:2014-06-28
  • 通讯作者: 吴映璇,Tel:(020)38290337,E-mail:allanwyx@126.com
  • 基金资助:

    广东省科技计划项目（2015A030401074，2014A040401064）.

Simultaneous determination of monepantel and its metabolite residues in cow and sheep milk by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

WU Yingxuan, XIE Minling, YAO Yangxun, LAN Cao   

  1. Guangdong Inspection and Quarantine Technology Center, Key Laboratory of Animals and Plants and Food Import and Export of Technical Measures in Guangdong Province, Guangzhou 510623, China
  • Received:2018-03-15 Online:2018-08-08 Published:2014-06-28
  • Supported by:

    Science and Technology Project of Guangdong Province (Nos.2015A030401074, 2014A040401064).

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摘要：

建立了高效液相色谱-串联质谱快速测定牛奶和羊奶中莫奈太尔及其代谢产物残留量的分析方法。样品经乙腈沉淀蛋白质，中性氧化铝固相萃取柱净化，以Inertsil C8-3（150 mm×4.6 mm，5 μm）色谱柱分离，甲醇-乙酸铵溶液为流动相进行梯度洗脱，采用电喷雾负离子监测模式检测，外标法定量。结果表明，在0.1~5.0 μg/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0.99），定量限为2.0 μg/kg。莫奈太尔及其代谢产物在2类基质中3个水平（2.0、50和100 μg/kg）下的加标回收率为90.1%~103.3%，相对标准偏差（RSD）为2.0%~6.2%（n=6）。该方法操作简便、快速，灵敏度高，抗干扰能力强，回收率和重复性良好，能够满足牛奶和羊奶中莫奈太尔及其代谢产物残留量的检测要求。

关键词: 代谢产物, 高效液相色谱-串联质谱, 固相萃取, 莫奈太尔, 奶

Abstract:

A method for the rapid and simultaneous determination of monepantel and its metabolite residues in cow and sheep milk has been developed using high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile to precipitate the proteins and passed through a neutral alumina solid phase extraction (SPE) cartridge. The extracts were separated on an Inertsil C8-3 column (150 mm×4.6 mm, 5 μm) with a gradient elution program consisting of methanol and ammonium acetate. A triple stage quadrupole mass spectrometer equipped with an electrospray ionization source in negative ion mode was used to detect monepantel and its metabolite residues. The quantification of the analytes was performed by the external standard method. Good linear relationships between the peak areas and mass concentrations of the analytes were obtained in the range of 0.1-5.0 μg/L with correlation coefficients greater than 0.99 (n=6). The limits of quantification were 2.0 μg/kg. The recoveries of the analytes in cow and sheep milk at three spiked levels (2.0, 50, and 100 μg/kg) were in the range of 90.1%-103.3% with relative standard deviations between 2.0% and 6.2% (n=6). This method is fast, accurate, and highly sensitive, exhibits strong anti-interference capability with good recovery and repeatability, and can thus be used to simultaneously determine monepantel and its metabolite residues in cow and sheep milk.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), metabolites, milk, monepantel, solid phase extraction (SPE)

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