色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定动物组织中残留的10种β2-兴奋剂

吴平谷1,陈慧华2,王强3,应永飞2,赵永信1,宋国良1,徐小明1

  

  1. 1.Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310009, China;
    2.Zhejiang Provincial Inspection Center for Animal Products Quality, Hangzhou 310020, China;
    3.Zhejiang Provincial Agricultural Scientific Academy, Hangzhou 310020, China
  • 收稿日期:2007-07-10 修回日期:2007-09-27 出版日期:2008-01-30 发布日期:1984-09-25
  • 通讯作者: 吴平谷

Multi-residue analysis of 10 β2-agonists in animal tissues using gas chromatography-mass spectrometry

WU Pinggu1, CHEN Huihua2, WANG Qiang3, YING Yongfei2,
ZHAO Yongxin1, SONG Guoliang1, XU Xiaoming1

  

  1. 1.Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310009, China;
    2.Zhejiang Provincial Inspection Center for Animal Products Quality, Hangzhou 310020, China;
    3.Zhejiang Provincial Agricultural Scientific Academy, Hangzhou 310020, China
  • Received:2007-07-10 Revised:2007-09-27 Online:2008-01-30 Published:1984-09-25
  • Contact: Wu Pinggu

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摘要：

采用同位素稀释法并结合固相萃取技术,建立了动物组织中马布特罗、特布他林、卡布特罗、克伦特罗、西马特罗、沙丁胺醇、clenpenterol、苯氧丙酚胺、班布特罗、莱克多巴胺等10种β2-兴奋剂残留的气相色谱-质谱(GC-MS)检测方法。动物组织中添加同位素内标D9-克伦特罗、D3-沙丁胺醇、D5-莱克多巴胺,经无水乙醇提取、正己烷脱脂、SLS离子交换固相萃取柱净化后，用双三甲基硅基三氟乙酰胺+1%三甲基氯硅烷衍生，再进行GC-MS测定,内标法定量。结果表明,动物组织中添加2.0～10.0 μg/kg水平的β2-兴奋剂,回收率为72.8%~110.3%,相对标准偏差为1.2%~11.3%,最低检测限为0.5～1.0 μg/kg。

关键词: β2-兴奋剂, 动物组织 , 固相萃取, 气相色谱-质谱法, 同位素稀释

Abstract:

A method for multi-residue analysis of β2-agonists, mabuterol, terbutaline, carbuterol, clenbuterol, cimaterol, salbutamol, clenpenterol, isoxsuprine, bambuterol and ractopamine in animal tissues using gas chromatography-mass spectrometry, based on isotope dilution and solid phase extraction has been developed. The homogenized sample was spiked with isotope-labeled internal standards, D9-clenbuterol, D3-salbutamol and D5-ractopamine, extracted with anhydrous alcohol, defatted using hexane, and cleaned-up on an SLS cartridge, and derivatized with N,O-bis(trimethylsilyl)trifluoro acetamide （BSTFA）+1%trimethylchlorosilane （TMCS）. The experimental results indicated that the recoveries were 72.8%-110.3%, and the relative standard deviations were 1.2%-11.3% in blank samples spiked with the above mentioned agonists at 2.0-10.0 μg/kg, and the corresponding detection limits were 0.5-1.0 μg/kg.

Key words: animal tissues , isotope dilution, solid phase extraction, β2-agonists, gas chromatography-mass spectrometry (GC-MS)