食品科学 ›› 2012, Vol. 33 ›› Issue (16): 159-162.

• 分析检测 • 上一篇    下一篇

亲水作用色谱串联质谱同时检测食品接触产品中三聚氰胺和三聚氰酸单体迁移量

吕水源1,井 伟1,2,李小晶1,*,江晓芬1,刘正才1,唐 熙1,陈旻实1,陈锦权2   

  1. 1.福建出入境检验检疫局检验检疫技术中心 2.福建农林大学食品科学学院
  • 收稿日期:2011-06-02 修回日期:2012-06-06 出版日期:2012-08-25 发布日期:2012-09-07
  • 通讯作者: 李小晶 E-mail:lxjciq@hotmail.com
  • 基金资助:

    福建省科技计划重点项目;福建出入境检验检疫局科技计划项目

Simultaneous Determination of Melamine and Cyanuric Acid in Food Contact Packaging Materials by Hydrophilic Liquid Chromatography-Tandem Mass Spectrometry

  • Received:2011-06-02 Revised:2012-06-06 Online:2012-08-25 Published:2012-09-07

摘要: 建立一种亲水作用色谱串联质谱技术同时检测食品接触产品中三聚氰胺与三聚氰酸单体迁移量的方法。样品采用水、体积分数4%乙酸溶液、体积分数10%乙醇溶液、异辛烷和橄榄油模拟物进行浸泡。在优化色谱及质谱条件下三聚氰胺和三聚氰酸能很好分离,且分别在1~100ng/mL和2~200ng/mL范围内,峰面积和质量浓度线性关系良好。在50ng/mL添加回收实验结果表明,三聚氰胺和三聚氰酸的平均回收率分别为86.2%~134.0%和78.9%~156.0%,相对标准偏差分别为6.44%~17.93%和5.95%~11.78%。该法简便、快速、准确,可同时测定食品接触产品中三聚氰胺与三聚氰酸单体迁移量。

关键词: 亲水作用色谱串联质谱, 食品接触产品, 三聚氰胺, 三聚氰酸, 迁移

Abstract: An HILC-MS/MS method was developed to simultaneously determine melamine and cyanuric acid in food contact packaging materials. Samples were extracted with H2O, 4% acetic acid (V/V), 10% ethanol isooctane (V/V) and olive oil separately, kept in a 70 ℃ incubator for 2 h and then filtered through a 0.2 μm microporous membrane prior to injection into an HILC-MS/MS system. Melamine and cyanuric acid were separated, identified and quantified on HILC column by gradient mobile phase and monitored in a positive/negative electrospray ionization and multiple reaction monitor (MRM) mode. A good linear range was achieved over the concentration range of 1-100 ng/mL and 2-200 ng/mL for melamine and cyanuric acid in different stimulants, respectively. The limits of detection and limits of quantification were in the range of 0.4-0.8 ng/mL. The recovery rates of melamine and cyanuric acid were 134.0%-86.2% and 156.0%-78.9% with RSDs of 6.44%-17.93% and 5.95%-11.78%. This method was simple, rapid, and accurate, and suitable for the determination of melamine and cyacuric acid in food contact packaging materials.

Key words: HILC-MS/MS, food contact packaging materials, melamine, cyanuric acid, migration

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