中国农业科学 ›› 2009, Vol. 42 ›› Issue (3): 989-995 .doi: 10.3864/j.issn.0578-1752.2009.03.030

• 贮藏·保鲜·加工 • 上一篇    下一篇

辐解产物2-十二烷基环丁酮的测定方法

  

  1. 中国农业科学院农产品加工研究所/农业部辐照产品质量监督检验测试中心
  • 收稿日期:2007-11-19 修回日期:2008-09-28 出版日期:2009-03-10 发布日期:2009-03-10
  • 通讯作者: 哈益明

Determination of 2-Dodecylcyclobutanone in Irradiated Products

  

  1. 中国农业科学院农产品加工研究所/农业部辐照产品质量监督检验测试中心
  • Received:2007-11-19 Revised:2008-09-28 Online:2009-03-10 Published:2009-03-10
  • Contact: HA Yi-ming

摘要:

【目的】建立1种含脂辐照食品中特异性辐解产物2-十二烷基环丁酮的萃取分离以及定量分析的新方法。【方法】采用硅胶层析柱萃取分离、气相色谱-质谱联用检测,对淋洗剂浓度、硅胶活化程度、收集时间及气相色谱-质谱条件等技术参数进行优化。【结果】该方法对2-十二烷基环丁酮标准品的最低检出限为0.005 mg?L-1,0.1~2.0 mg?L-1的添加回收率为75.9%~103.9%,相对标准偏差(RSD)均小于5.7%。【结论】与欧盟标准方法EN1785进行比较,硅胶柱分离法具有成本低、提取效率高、重现性好、检出限低、承载样品量大等优点。

关键词: 2-十二烷基环丁酮, 辐照, 硅胶柱, 气相色谱-质谱联用

Abstract:

【Objective】 A novel method was developed for quantitative determination of 2-dodecylcyclobutanone which is one of the specific markers of irradiated fat containing foods. 【Method】 The method includes extraction and separation by silica gel column and analysis by capillary column gas chromatography-mass spectrometry (GC-MS). And the correlative parameters of the concentration of eluting solvent, extent of deactivated silica, and collecting time for separation and chromatogram detection were optimized. 【Result】The limit of detection was 0.005 mg?L-1, the recoveries were 75.9%-103.9% according to adding concentration of 0.1-2.0 mg?L-1, and the relative standard deviations were all below 5.7%. 【Conclusion】It showed that the silica gel column separation method has lower cost, higher separative efficiency, better stability, lower detection limit, and larger analytic sample as compared to the EN1785 method.

Key words: 2-dodecylcyclobutanone, irradiation, silica column, gas chromatography-mass spectrometry