食品科学 ›› 2012, Vol. 33 ›› Issue (2): 231-234.doi: 10.7506/spkx1002-6630-201202051

• 分析检测 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱法测定食品中的丙烯酰胺

程 雷,郑炎夏,徐 虹,孙宝国   

  1. 北京工商大学 食品添加剂与配料北京高校工程研究中心,食品风味化学北京市重点实验室
  • 出版日期:2012-01-25 发布日期:2012-01-16
  • 基金资助:
    北京市留学人员科技活动择优资助项目(201009); 北京市属高等学校科学技术与研究生创新工程建设项目(PXM2011_014213_113634); 北京工商大学2011 年本科生科学研究计划项目

Determination of Acrylamide in Foods by Solid-phase Extraction and HPLC-MS/MS

CHENG Lei,ZHENG Yan-xia,XU Hong,SUN Bao-guo   

  1. Beijing Key Laboratory of Flavor Chemistry, Beijing Higher Institution Engineering Research Center of Food Additives and Ingredients, Beijing Technology and Business University, Beijing 100048, China
  • Online:2012-01-25 Published:2012-01-16

摘要: 建立高效液相色谱-串联质谱仪测定食品中丙烯酰胺含量的方法。以[D3]-丙烯酰胺为同位素内标,使用20mg/mL淀粉酶溶液对样品进行酶解,经水浴、除脂、离心,利用固相萃取柱进行净化并浓缩后,通过高效液相色谱-串联质谱仪以多选择反应监测模式进行分析测定。该方法的检出限和定量限分别为4.8μg/kg和16.5μg/kg。本方法具有操作方便、准确率高、重复性好等优点,可广泛应用于各类食品中丙烯酰胺含量的检测。

关键词: 高效液相色谱-串联质谱, 固相萃取, 丙烯酰胺, 同位素内标

Abstract: A method using [D3]-acrylamide as an isotope internal standard for determining acrylamide in foods was established by solid-phase extraction coupled with high performance liquid chromatography and quadrupole tandem mass spectrometry (HPLC-MS/MS). Analytical procedures were composed of amylase hydrolysis at a concentration of 20 mg/mL, the removal of fat, cleanup by solid-phase extraction (SPE) and the determination by HPLC-MS/MS with a multi-reaction monitoring (MRM) mode and the addition of an internal standard. The limit of detection (LOD) and limit of quantitation (LOQ) of the developed method were 4.8 and 16.5μg/kg, respectively. This method has the advantages of convenient operation, high sensitivity, excellent accuracy and good reproducibility and is therefore suitable for the determination of acrylamide in foods.

Key words: high performance liquid chromatography and quadrupole tandem mass spectrometry (HPLC-MS/MS), solid phase extraction, acrylamide, isotope internal standard

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