色谱 ›› 2013, Vol. 31 ›› Issue (10): 1021-1027.DOI: 10.3724/SP.J.1123.2013.03019

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定粮食及肉制品中的24种工业染料

冯月超, 贾丽, 何亚荟, 王建凤, 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
  • 收稿日期:2013-03-07 修回日期:2013-04-26 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 贾丽
  • 基金资助:

    北京市科技专项项目(Z111106055311093).

Simultaneous determination of 24 industrial dyes in grain and meat products by ultra performance liquid chromatography-tandem mass spectrometry

FENG Yuechao, JIA Li, HE Yahui, WANG Jianfeng, LIU Yan, FAN Xiaojing   

  1. Beijing Centre for Physical and Chemical Analysis, Beijing Engineering Research Center of Food Safety Analysis, Beijing 100089, China
  • Received:2013-03-07 Revised:2013-04-26 Online:2013-10-28 Published:2013-10-08

摘要:

建立了测定粮食及肉制品中24种禁用工业染料的超高效液相色谱-串联质谱法。样品经甲醇、乙腈提取后,过WAX固相萃取柱净化。采用ACQUITY UPLC BEH C18分析柱分离,以10 mmol/L乙酸铵-0.2%甲酸水溶液和甲醇-乙腈(7:3, v/v)为流动相梯度洗脱,多反应监测(MRM)模式测定。24种染料的相关系数R2均大于0.99,回收率在61%~116%之间,方法的精密度(RSD, n=6)小于13%,定量限在0.1~4.0 μg/kg。该方法灵敏度高,操作简单、高效,适合于粮食及肉制品中24种禁用工业染料的同时定量及确证分析。

关键词: 超高效液相色谱-串联质谱, 工业染料, 固相萃取, 粮食, 肉制品

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analytical method was established for the simultaneous determination of 24 forbidden industrial dyes in grain and meat products. The sample was extracted with methanol and acetonitrile, and cleaned-up by a WAX solid phase extraction column. The solution was separated on an ACQUITY UPLC BEH C18 column eluted with a mixture of 10 mmol/L ammonium acetate-0.2%formic acid aqueous solution and methanol-acetonitrile (7:3, v/v) as the mobile phases, and then analyzed in multiple reaction monitoring (MRM) mode. The correlation coefficients were above 0.99, the average recoveries were 61%-116%, and the relative standard deviations (RSD, n=6) were lower than 13%. The quantification limits were 0.1-4.0 μg/kg. This method is simple, effective, sensitive, and suitable for the determination and confirmation of the 24 forbidden industrial dyes in grain and meat products.

Key words: grain, industrial dyes, meat products, solid phase extraction (SPE), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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