色谱

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气相色谱-串联质谱法测定食品中的三聚氰胺

卢业举,舒勇,赵成仕   

  1. National Center for Quality Supervision and Test of Agricultural-Avocation Processed Food, Hefei 230051, China
  • 收稿日期:2008-10-08 修回日期:2008-11-08 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 卢业举
  • 基金资助:

Determination of melamine residue in foods using gas chromatography-tandem mass spectrometry

LU Yeju, SHU Yong, ZHAO Chengshi   

  1. National Center for Quality Supervision and Test of Agricultural-Avocation Processed Food, Hefei 230051, China
  • Received:2008-10-08 Revised:2008-11-08 Online:2008-11-30 Published:1983-06-25
  • Contact: LU Yeju

摘要: 建立了使用气相色谱-串联质谱(GC-MS/MS)测定食品中三聚氰胺含量的分析方法。利用三氯乙酸超声萃取样品中的三聚氰胺,经乙酸锌溶液沉淀蛋白质后,将提取液离心、过滤、净化、衍生后采用GC-MS/MS的多反应监测模式(MRM)进行检测。方法的重现性良好,6次重复测定的峰面积的相对标准偏差小于9%;最低定量检测限(S/N=10)为1 μg/kg,在0.1~100 μg/L范围内具有良好的线性关系。应用所建立的方法测定了奶粉、奶糖、含乳饮料、饼干等食品中的三聚氰胺含量,为三聚氰胺滥用的检测和判断提供了方法。

关键词: 饼干 , 含乳饮料, 奶粉, 奶糖, 气相色谱-串联质谱法, 三聚氰胺

Abstract: A method of gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for melamine residue in foods. The sample was extracted under ultrasonication with trichloroacelic acid (TCA), the protein in the sample was precipitated with zinc acetate solution. The extract was centrifuged, filtered, purified, derivatized and detected using GC-MS/MS in multiple-reaction monitoring mode. The limit of detection for melamine was 1 μg/kg. The good linearity in the range of 0.1-100 μg/L was obtained. The relative standard deviation (RSD) of peak area was less than 9%. This method has been applied to the analysis of melamine in milk powder, toffee, milk beverages, biscuits and other foods. It provides a method for the detection of abuse of melamine.

Key words: biscuits , melamine, milk beverages, milk powder, toffee, gas chromatography-tandem mass spectrometry (GC-MS/MS)