食品科学 ›› 2010, Vol. 31 ›› Issue (6): 235-238.doi: 10.7506/spkx1002-6630-201006056

• 分析检测 • 上一篇    下一篇

固相萃取- 高效液相色谱检测法测定食用菌中三聚氰胺残留量

王登飞,黄智辉,郑俊超,陈练洪,王瑞龙   

  1. 漳州出入境检验检疫局
  • 收稿日期:2009-04-07 修回日期:2009-10-22 出版日期:2010-03-15 发布日期:2010-12-29
  • 通讯作者: 王登飞 E-mail:wdf117@sohu.com

Determination of Melamine Residue in Edible Fungi by Solid Phase Extraction and High Performance Liquid Chromatography

WANG Deng-fei,HUANG Zhi-hui,ZHENG Jun-chao,CHEN Lian-hong,WANG Rui-long   

  1. (Zhangzhou Entry-Exit Inspection and Quarantine Bureau, Zhangzhou 363000, China)
  • Received:2009-04-07 Revised:2009-10-22 Online:2010-03-15 Published:2010-12-29
  • Contact: WANG Deng-fei E-mail:wdf117@sohu.com

摘要:

建立食用菌中三聚氰胺的固相萃取- 高效液相色谱检测法。样品经三氯乙酸、乙腈提取,离心,混合型固相萃取小柱净化后,过0.45μm 滤膜,用配有二极管阵列检测器(PAD)的液相色谱仪检测,外标法定量。同时,以三聚氰胺标准品进行添加回收率测定,结果显示,本方法对三聚氰胺的测定低限为2.0mg/kg,回收率为81.3%~91.7%,测定的相对标准偏差均不大于5.6%。本方法能满足食用菌中三聚氰胺残留量常规检测的需要。

关键词: 固相萃取, 食用菌, 三聚氰胺, 残留量

Abstract:

A novel method based on solid phase extraction followed by high performance liquid chromatography (HPLC) was developed for the analysis of melamine residue in edible fungi. Samples were extracted with a mixed system composed of trichloroacetic acid and acetonitrile (3:1, V/V), cleaned up on mixed-mode SPE column and filtrated through 0.45 μm pore size membrane prior to analysis using a HPLC system equipped with PAD. Melamine was quantified by external standard method. The method exhibited a limit of detection of 2.0 mg/kg and a spike recovery range of 81.3% to 91.7% at three levels, with relative standard deviations (RSDs) of not more than 5.6%. The method proves to be most suitable for the determination of melamine residue in edible fungi.

Key words: solid phase extraction, aquatic products, melamine, residue

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