色谱

色谱

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液相色谱-串联质谱法测定鸡肌肉组织中的四环素类药物残留

刘艳华,张纯萍,门立强,刘智宏,王树槐

  

  1. China Institute of Veterinary Drug Control, Beijing 100081, China
  • 收稿日期:2005-03-18 修回日期:2005-11-21 出版日期:2006-03-30 发布日期:1987-06-25
  • 通讯作者: 刘艳华

Determination of Tetracycline Antibiotics Residues in Chicken Muscle by Liquid Chromatography-Tandem Mass Spectrometry

LIU Yanhua, ZHANG Chunping, MEN Liqiang, LIU Zhihong, WANG Shuhuai

  

  1. China Institute of Veterinary Drug Control, Beijing 100081, China
  • Received:2005-03-18 Revised:2005-11-21 Online:2006-03-30 Published:1987-06-25
  • Contact: LIU Yanhua

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摘要：

建立了一种专属、灵敏的方法,用于同时检测鸡肌肉组织中土霉素、四环素和金霉素的残留。首先对鸡肌肉组织中的四环素类药物进行提取,再经C18固相萃取柱净化,采用电喷雾离子源,以正离子检测方式进行质谱分析。实验结果表明，在25～500 μg/L这一质量浓度范围内上述3种四环素类药物均呈线性,其相关系数r＞0.99。在低、中、高3个质量浓度添加水平，3种四环素类药物的平均回收率为72.4%～94.9%,相对标准偏差小于11%。3种四环素类药物的检测限均可达到10 μg/kg。其方法学考察符合农牧发［2003］1号文件的有关规定。

关键词: 鸡肌肉组织 , 金霉素, 四环素, 土霉素, 液相色谱-串联质谱法

Abstract:

A sensitive and selective method is presented for simultaneous determination of tetracycline antibiotics (TCs) veterinary drugs. Oxytetracycline (OTC), tetracyclines (TC) and chlortetracycline (CTC) in the chicken muscle were extracted, and then solid-phase cleaned-up on a C18 reversed-phase column to obtain an extract suitable for analysis by liquid chromatography-tandem mass spectrometry（LC-MS/MS）. Electrospray ionization was applied and operated in the positive ion mode. The calibration curves were good linear between the peak areas and the mass concentrations of TCs from 25 to 500 μg/L with the correlation coefficient more than 0.99. The average recoveries from spiked chicken muscle at the three concentrations of 50, 100 and 200 μg/kg were from 72.4% to 94.9% with relative standard deviation less than 11%. The detection limits of TCs were 10 μg/kg. The method was successfully validated for chicken muscle in compliance with the requirements set by Document No.1 of 2003 dispatched by the Bureau of Animal Husbandary of Ministry of Agriculture. This method is suitable for the determination of OTC,TC and CTC in chicken muscle.

Key words: chichen muscle
, chlortetracycline, oxytetracycline, tetracyclines, liquid chromatography-tandem mass spectrometry（LC-MS/MS）