基于顶空固相微萃取-全二维气相飞行时间质谱快速检测烟草挥发性及半挥发性生物碱  

Rapid analysis of volatile and semi-volatile alkaloids in tobacco by headspace solid-phase microextraction combined with GC×GC-TOFMS

作　　者：向章敏 蔡凯 张婕 葛永辉 周淑平 郭玉双 耿召良 

机构地区：[1]贵州省烟草科学研究院,贵阳550081

出　　处：《分析试验室》2014年第11期1249-1254,共6页Chinese Journal of Analysis Laboratory

基　　金：贵州省烟草专卖局(公司)项目(201112;201307和201406);国家自然科学基金项目(31360431);贵州省科学技术基金项目(黔科合J字[2011]2143)资助

摘　　要：通过正交试验设计与单因素试验设计相结合,建立了顶空固相微萃取-全二维气相飞行时间质谱快速分析烟草挥发性及半挥发性生物碱的方法。烟叶样品在70℃条件下平衡20 min,然后采用PDMS/DVB/CAR纤维头在顶空瓶中平衡15 min,最后在250℃进样口解析3 min效果最好。以喹啉为内标,分别对烟草中烟碱、麦斯明和二烯烟碱3种生物碱的挥发性成分进行定性定量分析,其方法的线性相关系数（r^2）为0.9944-0.9992,检出限为0.60-150 pg,添加回收率为86.7%-98.3%,相对标准偏差为1.8%-4.2%。通过实际烟草样品检测表明,不同生物碱的挥发性与总量具有显著相关性。A rapid and accurate headspace solid-phase microextraction （SPME） combined with comprehensive two-dimensional gas chromatography-time of flight mass spectrometry （ GC × GC-TOFMS） for analysis of volatile and semi-volatile alkaloids in tobacco was established by orthogonal and single factor design. The optimized method included a headspace temperature of 70 ℃ for 20 min, an extraction time of 15 min for polydimethylsiloxane/divinylbenzene/carboxen （PDMS/DVB/CAR） and desorption time of 3 min at 250 ℃. As a result, the three alkaloids including nicotine, myosmine and nicotyrine were determined qualitatively and quantitatively by using quinoline as the internal standard, and linear range （ R^2 ） of this method was 0. 9944 - 0. 9992, and limits of detection （LOD） were 0. 60 - 150 pg. Meanwhile, the average recoveries of volatile and semi-volatile alkaloids in tobacco samples were in the range of 86. 7% - 98.3% with relative standard deviations （RSD） of 1.8% - 4. 2%. Finally, the developed analytical method was applied to revealing the relationship between volatility of alkaloids and amounts, and significant correlation was obtained.

关 键 词：固相微萃取 全二维气相飞行时间质谱 烟草 挥发性及半挥发性生物碱 快速检测 

分 类 号：O657.63[理学—分析化学]