食品科学 ›› 2009, Vol. 30 ›› Issue (14): 167-170.doi: 10.7506/spkx1002-6630-200914031

• 分析检测 • 上一篇    下一篇

超高效液相色谱- 串联质谱法快速检测鳗鱼中磺胺类、喹诺酮类、四环素族抗生素药物残留

刘正才,杨 方,余孔捷,李耀平,林永辉,张 琼,刘素珍   

  1. 福建出入境检验检疫局
  • 收稿日期:2008-10-20 出版日期:2009-07-15 发布日期:2010-12-29
  • 通讯作者: 刘正才 E-mail:zhengcailiu@yahoo.com.cn
  • 基金资助:

    国家质量监督检验检疫总局科技计划项目(2007IK147);福建省科技计划重点项目(2007Y001)

Simultaneous Determination of Qunolones, Sulfonamides and Tetracyclines Residues in Eel Using Solid Phase Extraction (SPE) and Ultra-performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry (UPLC-MS-MS)

LIU Zheng-cai,YANG Fang,YU Kong-jie,LI Yao-ping,LIN Yong-hui,ZHANG Qiong,LIU Su-zhen   

  1. Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China
  • Received:2008-10-20 Online:2009-07-15 Published:2010-12-29
  • Contact: LIU Zheng-cai, E-mail:zhengcailiu@yahoo.com.cn

摘要:

建立鳗鱼中15 种磺胺、3 种喹诺酮类以及4 种四环素族抗生素残留的超高效液相色谱- 串联质谱同时测定方法。采用酸性EDTA-Mcllvaine 缓冲液提取,经HLB 固相萃取小柱富积、净化后进行UPLC 分离,电喷雾串联质谱进行检测,多离子反应监测(MRM)模式定量。添加水平为5、10、20μg/kg 时各种化合物的平均回收率范围为72.4%~97.3%,RSD 值均小于14.4%。该法简单、快速、灵敏,适用于鳗鱼中多磺胺组分、喹诺酮及四环素族组分残留的同时测定。

关键词: 超高效液相色谱串联质谱法(UPLC/MS/MS), 磺胺类, 喹诺酮类, 四环素族, 鳗鱼

Abstract:

A robust and sensitive UPLC-MS-MS method was developed for the simultaneous determination of residues of 15 sulfonamides, 3 fluoroquinolones and 4 tetracylines in eel. The target compounds were extracted with acidic EDTA-Mcllvaine buffer solution, and enriched and cleared up using a hydrophilic-lipophilic balance (HLB) SPE cartridge. After seperation on UPLC BEH C18, the analytes were detected using a tandem mass spectrometry and quantified in multiple reaction monitoring (MRM) mode. At the spike levels of 5, 10 and 20 μg/kg respectively, the average recoveries for all the compounds were 72.4%-97.3%, and the variation coefficients were all under 14.4%. This method is simple, fast, sensitive, and particular for the simulaneous determination of sulfonamides, fluoroquinolones and tetracylines in eel.

Key words: ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS), sulfonamides, qunolones, tetracycline, eel

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