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两种气相色谱法测定辐照花生仁中挥发性碳氢化合物的研究

ISSN号：1004-4957
期刊名称：《分析测试学报》
时间：0
分类：O657.71[理学—分析化学;理学—化学] TQ413.21[化学工程]
作者机构：[1]中国农业科学院农产品加工研究所,北京100193
相关基金：中国农业科学院基本科研业务费专项资助项目（0032010027）; 农业部农业公益性行业科研专项资助项目（200803034）

关键词：碳氢化合物, 固相微萃取, 标识物, 气相色谱(GC), 花生仁, hydrocarbons, SPME, markers, GC, peanut kernel

中文摘要：

通过对花生仁辐照前后碳氢化合物类型与浓度差异的分析,建立了判别花生仁是否经过辐照的两种气相色谱鉴定方法,即弗罗里硅土柱层析-气相色谱-火焰离子化检测方法（Florisil柱层析-GC-FID）和顶空-固相微萃取-气相色谱-质谱（HS-SPME-GC-MS）检测方法。采用添加回收率实验,比较了两种方法对花生仁中3种主要的脂肪酸（棕榈酸、硬脂酸和油酸）辐解产生的6种碳氢化合物1-十四烯（1-C14∶1）、正十五烷（C15∶0）、1-十六烯（1-C16∶1）、正十七烷（C17∶0）、1,7-十六二烯（1,7-C16∶2）和8-十七烯（8-C17∶1）的检测效果。研究结果表明,Florisil柱层析-GC-FID法更适合于碳氢化合物的定量分析,6种碳氢化合物的添加回收率为84%~119%,RSD为1.1%~7.5%,但方法的前处理过程较复杂。HS-SPME-GC-MS法操作简便,能对花生仁中的标识性碳氢化合物进行准确快速的定性分析,但6种碳氢化合物的回收率较低,而RSD值较高。研究表明,1,7-C16∶2和8-C17∶1是辐照花生仁形成的特异性辐解产物,其中1,7-C16∶2浓度增加最为显著,是鉴定辐照花生的最佳标识物。

英文摘要：

Two methods,including Florisil column chromatography-gas chromatography-flame ionization detector（Florisil column chromatography-GC-FID）and headspace-solid phase microextraction-gas chromatography-mass spectrum（HS-SPME-GC-MS）were developed to identify irradiated peanut kernel by analysis of differences of types and contents of hydrocarbons between unirradiated and irradiated samples.The recoveries and RSDs of six hydrocarbons,e.g.1-tetradecene（1-C14∶1）,n-pentadecane（C15∶0）,1-hexadecene（1-C16∶1）,n-heptadecane（C17∶0）,1,7-hexadecadiene（1,7-C16∶2）and 8-heptadecene（8-C17∶1）,produced by three main fatty acids（palmitic acid,stearic acid and oleic acid） in peanut kernel,were compared.The results showed that Florisil column chromatography-GC-FID method was more suitable for quantitative analysis.The recoveries of the six hydrocarbons were between 84% and 119% with RSDs of 1.1%-7.5%.However,the pretreatment procedure of this method was complicated.HS-SPME-GC-MS method could be used for the exactly and quickly qualitative analysis of hydrocarbons in peanut kernel for its simple procedure,but it was not good at quantitative analysis for its low recoveries and high RSDs.Four hydrocarbons 1-C14∶1,C15∶0,1-C16∶1 and C17∶0,were detected in unirradiated peanut kernel.Only 1,7-C16∶2 and 8-C17∶1 were special radialytic products in irradiated peanut kernel,in which 1,7-C16∶2 was selected as the best markers of irradiated peanuts since its contents had big differences between the unirradiated sample and the irradiated ones.

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