色谱

色谱

• 研究论文 • 上一篇    下一篇

超高效液相色谱-电喷雾串联质谱法测定饲料中残留的三聚氰胺

蔡勤仁,欧阳颖瑜,钱振杰,彭玉芬

  

  1. Technical Center of Zhuhai Entry-Exit Inspection and Quarantine Bureau, Zhuhai 519015, China
  • 收稿日期:2007-08-21 修回日期:2007-10-23 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 蔡勤仁

Determination of melamine residue in feeds by ultra performance liquid chromatography coupled with
electrospray　tandem mass spectrometry

CAI Qinren, OUYANG Yingyu, QIAN Zhenjie, PENG Yufen   

  1. Technical Center of Zhuhai Entry-Exit Inspection and Quarantine Bureau, Zhuhai 519015, China
  • Received:2007-08-21 Revised:2007-10-23 Online:2008-05-30 Published:1984-03-25
  • Contact: CAI Qinren

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摘要：

饲料样品经1%三氯乙酸-二甲基亚砜提取,Waters Oasis MCX柱净化,超高效液相色谱分离,最终采用电喷雾串联四极杆质谱进行检测。结果表明,三聚氰胺在饲料中的含量范围为10～5000 μg/kg时,线性关系良好(r＞0.99)。在10～100 μg/kg 的添加水平范围内的平均回收率为83%～94%,相对标准偏差为4.2%～6.5%。该方法的检出限为10 μg/kg。

关键词: 超高效液相色谱-串联质谱, 三聚氰胺, 饲料

Abstract:

A method for fast determination melamine residue in feeds was established. An ultra performance liquid chromatography coupled with electrospray ionization quadrupole tandem mass spectrometry (UPLC-ESI-MS/MS) was used. The residue was quantified with multiple reaction monitoring (MRM) mode. The method was validated and good results were obtained with respect to precision, repeatability and spiked recovery. The limit of detection was 10 μg/kg for melamine, and the linear range was from 10 to 5000 μg/kg. The average recoveries were between 83% and 94% in the spiked range of 10-100 μg/kg, and the relative standard deviations (RSDs) were between 4.2% and 6.5%. The method has good repeatability and high sensitivity, and can be applied for the determination of melamine residue in feeds.

Key words: feed
, melamine, ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS)