食品科学

• 分析检测 • 上一篇    下一篇

固相萃取-液质联用法同时测定食品中11种禁用工业染料

冯月超,何亚荟,王建凤,贾 丽,杨志超,刘 艳,范筱京   

  1. 北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心,北京 100089
  • 出版日期:2013-12-25 发布日期:2014-01-03

Simultaneous Determination of 11 Industrial Dyes in Foods by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Feng Yue-chao,HE Ya-hui,WANG Jian-feng,JIA Li,YANG Zhi-chao,LIU Yan,FAN Xiao-jing   

  1. Beijing Engineering Research Center of Food Safety Analysis, Beijing Center for Physical and Chemical Analysis, Beijing 100089, China
  • Online:2013-12-25 Published:2014-01-03

摘要:

采用固相萃取净化技术、固相萃取-液质联用分离和测定粮食及肉制品中苏丹红G、苏丹蓝2、苏丹红7B、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、对位红、分散橙1、分散橙11、分散橙37共11种禁用工业染料。样品经正己烷提取,中性氧化铝固相萃取柱净化,采用C18柱,以10mmol/L乙酸铵-0.2%甲酸溶液(A)和甲醇-乙腈溶液(B)(7:3,V/V)为流动相,采用多反应监测(MRM)模式测定。11种染料的相关系数R2均大于0.99,回收率在70%~102%之间,方法精密度小于14%(RSD,n=6),检出限在0.02~0.8μg/kg。本方法灵敏度高、操作简单高效,适合于粮食及肉制品中11种禁用工业染料的定量及确证分析。

关键词: 固相萃取, 液质联用法, 食品, 工业染料

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) analysis method
was established for the simultaneous determination of 11 industrial dyes such as Sudan red G, Sudan blue 2, Sudan red 7B,
Sudan red Ⅰ, Sudan red Ⅱ, Sudan red Ⅲ, Sudan red Ⅳ, Para red, Disperse orange 1, Disperse orange 11, and Disperse
orange 37 in foods. Samples were extracted with n-hexane, and cleaned up sequentially by neutral alumina column and solid
phase extraction column. The separation was performed on an ACQUITY UPLC BEH C18 column, using a mixture of 0.2%
formic acid in water with 10 mmol/L ammonium acetate and methanol-acetonitrile (7:3,V/V) as the mobile phase, and
then analyzed in the multiple reaction monitoring (MRM) mode.The correlation coefficients were above 0.99, the average
recoveries were 70%–102% with relative standard deviations (RSD, n = 6) lower than 14%. The limits of detection of the
method were 0.02–0.8 μg/kg. This UPLC-MS-MS method is simple, effective and sensitive, and can be suitable for the
determination and confirmation of residues of 11 bannedindustrial dyes in foods.

Key words: solid phase extraction, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MSMS), food, industrial dyes