食品科学

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超高效液相色谱-串联质谱法同时检测牛乳中4 种驱虫药物残留

侯改成1,谭艾娟2,*,吕世明3,金晓峰4,张剑勇4   

  1. 1.贵州大学药学院,贵州 贵阳 550025;2.贵州大学生命科学学院,贵州 贵阳 550025;
    3.贵州大学动物科学学院,贵州 贵阳 550025;4.贵州省兽药监察所,贵州 贵阳 550003
  • 出版日期:2015-03-25 发布日期:2015-03-17
  • 通讯作者: 谭艾娟
  • 基金资助:

    贵州省科技厅农业攻关课题(黔科合NZ字[2012]3011号);贵阳市农委科学技术计划项目(筑科合(2009第12-1号))

Simultaneous Determination of 4 Parasiticide Residues in Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

HOU Gaicheng1, TAN Aijuan2,*, LÜ Shiming3, JIN Xiaofeng4, ZHANG Jianyong4   

  1. 1.贵州大学药学院,贵州 贵阳 550025;2.贵州大学生命科学学院,贵州 贵阳 550025;
    3.贵州大学动物科学学院,贵州 贵阳 550025;4.贵州省兽药监察所,贵州 贵阳 550003
  • Online:2015-03-25 Published:2015-03-17
  • Contact: TAN Aijuan

摘要:

建立同时检测牛乳中4 种驱虫药物(吡喹酮、伊维菌素、阿维菌素、多拉菌素)残留的超高效液相色谱-串联质谱的方法。样品经乙腈提取,碱性氧化铝固相萃取小柱净化,采用UPLC ACQUITY BEH C18柱,以0.1%甲酸-乙腈(A)和0.1%甲酸-5.0 mmol/L乙酸铵(B)为流动相,梯度洗脱分离,在电喷雾正离子模式下以多反应监测方式检测。结果表明:4 种驱虫药物在5~100 ng/mL范围内线性良好,相关系数大于0.996,加标样品的平均回收率为76.4%~113.3%,相对标准偏差(n=6)为2.4%~10.6%。吡喹酮、伊维菌素、阿维菌素、多拉菌素的检出限分别为1.0、2.5、2.5、2.5 μg/kg。该方法简便、快速、准确,可以同时检测牛乳中吡喹酮、伊维菌素、阿维菌素、多拉菌素残留。

关键词: 超高效液相色谱-串联质谱, 吡喹酮, 阿维菌素类药物, 残留, 牛乳

Abstract:

A new multi-residue analytical method was developed for the simultaneous determination of residues of 4
parasiticides, i.e. praziquantel, ivermectin, abamectin and doramectin, in milk by ultra performance liquid chromatography
tandem mass spectrometry (UPLC-MS-MS). The samples were extracted with acetonitrile and then cleaned up with alkaline
alumina column. The target compounds were separated with UPLC ACQUITY BEH C18 column. The mobile phase A
(acetonitrile plus 0.1% formic acid) and the mobile phase B (0.1% formic acid plus 5 mmol/L ammonium acetate) were
used in a gradient elution program. The target drugs were detected by electrospray ionization mass spectrometry in positive
ion mode with multiple reaction monitoring. The results showed good linear relationships in the range of 5-100 ng/mL
and the correlation coefficients were all above 0.996. The average recoveries ranged from 76.4% to 113.3%, and the relative
standard deviations (RSDs) were in the range of 2.4%-10.6%. The limits of detection (LODs) for praziquantel, ivermectin,
abamectin and doramectin were 1.0, 2.5, 2.5, and 2.5 μg/kg, respectively. The method was simple, rapid, and accurate to measure
the residues of these four parasiticides praziquantel, ivermectin, abamectin and doramectin in milk.

Key words: UPLC-MS-MS, praziquantel, avermectins, residue, milk

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