色谱

色谱 ›› 2011, Vol. 29 ›› Issue (05): 404-408.DOI: 10.3724/SP.J.1123.2011.00404

• 研究论文 • 上一篇    下一篇

柱前衍生化-气相色谱-质谱法定量测定食品中丙烯酰胺的含量

杨斯超, 张慧, 汪俊涵, 陈芳*   

  1. 中国农业大学食品科学与营养工程学院, 农业部果蔬加工重点开放实验室, 果蔬加工教育部工程研究中心, 北京 100083
  • 收稿日期:2011-01-09 修回日期:2011-03-07 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 陈芳,博士,副教授,研究方向为农产品加工及贮藏
  • 基金资助:
    国家“十一五”科技支撑计划项目(2009BADB9B00).

Determination of bisphenol A in milk by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction of monodisperse magnetic submicron particles as adsorbent

YANG Sichao, ZHANG Hui, WANG Junhan, CHEN Fang*   

  1. College of Food Science & Nutritional Engineering, Key Laboratory of Fruits and Vegetables Processing of Ministry of Agriculture, Engineering Research Centre for Fruits and Vegetables Processing of Ministry of Education, China Agricultural University, Beijing 100083, China
  • Received:2011-01-09 Revised:2011-03-07 Online:2011-05-28 Published:2011-05-28

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824

被引次数

47

摘要： 建立了气相色谱-质谱(GC-MS)定量测定食品中丙烯酰胺含量的分析方法。选择13C3-丙烯酰胺作为内标物。通过超纯水提取食品中的丙烯酰胺,经正己烷脱脂两次后,在酸性条件下选用溴化钾/溴酸钾为衍生剂进行衍生化反应,再采用乙酸乙酯进行液-液萃取两次,最后用三乙胺将丙烯酰胺转化为更稳定的产物2-溴丙烯酰胺,利用质谱检测器在选择离子扫描模式下测定2-溴丙烯酰胺。该方法在0.05～2.00 mg/kg范围具有良好的线性(r2=0.9995);检出限和定量限分别达到3 μg/kg和7 μg/kg;回收率范围为62.7%～65.5%。通过与前期建立的液相色谱-串联质谱(HPLC-MS/MS)方法进行对比,该法在薯片和面包样品中丙烯酰胺的检测结果略偏高,是一种可以用于常见食品中丙烯酰胺含量测定的分析方法。

关键词: 丙烯酰胺, 气相色谱-质谱, 食品, 柱前衍生化

Abstract: Monodisperse magnetic submicron particles were synthesized by a solvothermal reduction method. A solid phase extraction (SPE) based on the monodisperse magnetic submicron particles and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of bisphenol A (BPA) at trace level in milk has been established. The important parameters that affect the extraction efficiency such as the solution pH, dosage of magnetic submicron particles, nature of elution solution and its volume were optimized. The optimal extraction conditions were as follows: the pH 6.0, the dosage of 3.5 mg magnetic submicron particles and 0.4 mL methanol as elution solution. BPA was analyzed by HPLC-MS/MS in negative ion mode using an Agilent XDB C18 column as analytical column. Under the optimal conditions, the calibration curves showed a good linearity in the BPA concentration range of 1.0~100.0 μg/L. The correlation coefficient was 0.9993. The average recoveries of BPA at three spiked levels ranged from 85.3% to 96.1% with the relative standard deviations (RSDs) less than 10%. The detection limit of the method was 1.0 μg/L. The method is sensitive, simple, and suitable for the rapid determination of BPA in milk.

Key words: bisphenol A (BPA), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), milk, monodisperse magnetic submicron particles, solid-phase extraction (SPE)