食品科学 ›› 2012, Vol. 33 ›› Issue (12): 190-195.doi: 10.7506/spkx1002-6630-201212038

• 分析检测 • 上一篇    下一篇

平行定量浓缩仪- 超高效液相色谱- 串联质谱联用快速检测鳗鱼中8 种喹诺酮类药物残留量

张宪臣1,华洪波2,张朋杰1,王 勇1,*,杨 芳1,李 蓉1,胡仪光1,卢俊文1   

  1. 1.中山出入境检验检疫局 2.中山市广外附设外语学校
  • 出版日期:2012-06-25 发布日期:2012-07-27
  • 基金资助:
    广东省自然科学基金项目(7301741);中山市科技计划项目(20103A235); 广东检验检疫局科技计划项目(2012GDK49)

Rapid Simultaneous Determination of Eight Quinolone Residues in Eel by Syncore Analyst-Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

ZHANG Xian-chen1,HUA Hong-bo2,ZHANG Peng-jie1,WANG Yong1,*,YANG Fang1,LI Rong1, HU Yi-guang1, LU Jun-wen1   

  1. (1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528403, China; 2. Zhongshan Foreign Language School Attached to Guangdong University of Foreign Studies, Zhongshan 528401, China)
  • Online:2012-06-25 Published:2012-07-27

摘要: 建立鳗鱼肉中8种奎诺酮残留量的平行定量浓缩仪-超高效液相色谱-串联质谱检测方法。以氘代试剂为内标,样品经酸化乙腈萃取后,平行定量浓缩仪浓缩,用正己烷脱脂,采用超高效液相色谱-串联质谱选择反应监测正离子模式测定,可同时对鱼肉中奎诺酮进行定性和定量。奎诺酮检出限可达0.5μg/kg,定量低限可达1.0μg/kg。在2.5~200ng/mL范围内峰强度与质量浓度的线性关系良好(r>0.99)。方法的平均回收率在81.4%~111.1%之间。方法简单、快速、稳定、准确、灵敏度高,适合于实验室大批量检测水产品样品。

关键词: 平行定量浓缩仪, 超高效液相色谱-串联质谱, 奎诺酮, 鳗鱼, 残留量

Abstract: A method for the simultaneous determination of eight quinolone residues in eel was developed by syncore analyst-ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (SA-UPLC-MS/MS). Deuterium substituted reagents were added as internal standards before sample extraction with acidified acetonitrile, followed by concentration using a Syncore Analyst and clean-up with hexane. Eight quinolone residues were analyzed by UPLC-MS/MS under positive ion mode. The limit of detection of the method for eight quinolones was 0.5μg/kg, and the limit of quantification was 1.0μg/kg. The calibration curves showed good linearity over the concentration range of 2.5-200 ng/mL (r > 0.99). The average recovery rates were 81.4%-11.1% across three spike levels (n = 6). This method was simple, rapid, stable, reliable, sensitive and suitable for the determination of bulk aquatic products.

Key words: Syncore Analyst, ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry, qunolones, eel, residues

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