辐解产物2-十二烷基环丁酮的测定方法

Determination of 2-Dodecylcyclobutanone in Irradiated Products

【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0.005mg·L-1,0.1～2.0mg·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。

[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 EN 1785 method.