食品科学

• 分析检测 • 上一篇    下一篇

凝胶渗透色谱-气相色谱-串联质谱法同时测定食品中3种抗氧化剂

曹淑瑞,徐 芬,张 雷,李贤良,王国民,明德旺,袁 若   

  1. 1.重庆出入境检验检疫局,重庆 400020;2.西南大学化学化工学院,重庆 400715
  • 出版日期:2013-06-25 发布日期:2013-06-17

Simultaneous Determination of 3 Antioxidants in Foods by Gas Chromatography-Tandem Mass Spectrometry Coupled with Gel Permeation Chromatography

CAO Shu-rui,XU Fen,ZHANG Lei,LI Xian-liang,WANG Guo-min,MING De-wang,YUAN Ruo   

  1. 1. Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing 400020, China;
    2. College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715, China
  • Online:2013-06-25 Published:2013-06-17

摘要:

建立凝胶渗透色谱结合气相色谱-串联质谱(GC-MS/MS)同时测定食品中3种抗氧化剂的定性、定量分析方法。样品经正己烷饱和的乙腈提取,凝胶渗透色谱仪净化后,在30m长的气相毛细管色谱柱上分离,GC-MS/MS以多反应离子监测方式(SRM)检测目标化合物。结果表明:该方法在0.05~10mg/L范围内线性关系良好,相关系数(r)大于0.99。添加质量浓度为0.5~2.0mg/L时,抗氧化剂的回收率为77.6%~95.4%,相对标准偏差为2.7%~8.5%。方法的检出限(LOD)为0.03~0.10mg/kg(以3倍性噪比计)。本方法具有提取效率高,净化效果好,准确灵敏等优点,适用于食品中多种抗氧化剂的检测。

关键词: 气相色谱-串联质谱, 凝胶渗透色谱, 抗氧化剂

Abstract:

A novel method has been established for the rapid separation and determination of 3 antioxidants (TBHQ, BHA and
BHT) in foods. The target analytes were extracted with hexane-saturated acetonitrile and the extract was purified by gel permeation
chromatography (GPC). The analytes were separated on a TR-35ms column (30 m × 0.25 mm, 0.25 μm) and detected by tandem
mass spectrometry with EI under multiple reaction-monitoring (MRM) mode. An excellent linearity (r > 0.99) was observed in
the concentration range of 0.05 to 10 mg/L for each antioxidant. The recovery rates ranged from 77.6% to 95.4% at three
levels of 0.5, 1.0 mg/L and 2.0 mg/L, with relative standard deviations (RSDs) of 2.7%-8.5%. The limits of detection were
0.03-0.1 mg/kg (n = 3) for these analytes. The established method is rapid, precise, sensitive, efficient and applicable for
the analysis of TBHQ, BHA and BHT in foods.

Key words: gas chromatography-tandem mass spectrometry, gel permeation chromatography, antioxidants