热脱附-冷阱系统-气相色谱-质谱法同时测定卷烟烟丝中7种生物碱和9种香精成分  

Thermal Desorption-Cooled Injection System-Gas Chromatography-Mass Spectrometry for Simultaneous Determination of Seven Kinds of Alkaloids and Nine Kinds of Flavor Compounds in Cigarette

作　　者：陈凤明 张峰[1] 高飞[1] 雍炜[1] 杨敏莉[1] 冯峰[1] CHEN Feng-Ming;ZHANG Feng;GAO Fei;YONG Wei;YANG Min-Li;FENG Feng(Institute of Food Safety,Chinese Academy of Inspection and Quarantine,Beijing 100176,China)

机构地区：[1]中国检验检疫科学研究院,北京100176

出　　处：《分析化学》2021年第1期128-136,共9页Chinese Journal of Analytical Chemistry

基　　金：中央级公益性科研院所基本科研业务费专项(No.2018JK001)资助。

摘　　要：建立了热脱附-冷阱系统-质谱技术(TDU-CIS-MS)同时检测卷烟烟丝中7种生物碱(尼古丁、降烟碱、新烟碱、麦斯明、二烯烟碱、异喹啉和2,3-联吡啶)和9种香精(二氢香豆素、香兰素、香豆素、乙基香兰素、甲基香兰素、7-甲基香豆素、7-甲氧基香豆素、7-乙氧基-4甲基香豆素和环香豆素)的分析方法。通过在线热脱附卷烟样品,优化了热脱附温度、热脱附时间、冷阱捕集管及温度以及吹扫时间等条件,使挥发的生物碱和香精化合物进入冷阱系统富集,以DB-5MS色谱柱分离,在选择离子监测模式(SIM)下,采用基质曲线外标法定量分析以消除基质效应。结果表明,7种生物碱和9种香精成分的线性检测范围为1~500μg/L,线性相关系数(R 2)均大于0.993,方法检出限为0.02~0.50μg/kg,定量限为0.10~2.0μg/kg。此方法样品前处理简单、安全、灵敏度和准确性高,适用于烟草中生物碱和香精成分的测定,对于加热不燃烧卷烟烟丝中复杂挥发性痕量物质成分的分析具有重要意义。A novel method for determination of seven kinds of alkaloids(isoquinoline,nicotine,3-(2-pyrrolidinyl)plridine nornicotine,myosmine,b-nicotyrine,Anabasine,2,3′-bipyridine,and anabaseine)and nine kinds of flavor compounds(hydrocoumarin,vanillin,coumadin,ethyl vanillin,methyl vanillin,7-methyl coumarin,7-methoxycoumarin,7-ethoxy-4-methylcoumarin,and pyranocoumarin)in cigarette by thermal desorption-cooled injection system coupled with gas chromatography-mass spectrometry(TDU-CIS-GC-MS)was developed.By optimizing the conditions such as TDU(time,temperature,and flow rate of helium gas),CIS temperature,vent time and purge time,the cigarette alkaloid compound could be completely thermal desorption,and the volatile alkaloids and coumarin substances were enriched using the cold injection system.A DB-5 MS chromatographic column was used for separation,and a matrix curve external label method was used to quantify the matrix effect under the selected ion monitoring mode(SIM).The results showed that the linear range of 7 kinds of alkaloids and 9 kinds of flavors was 1-500μg/L,the linear correlation coefficient(R 2)was greater than 0.993,and the limits of detection(LOD)and limits of quantitation(LOQ)were 0.02-0.50μg/kg and 0.1-2.0μg/kg,respectively.This method was simple,safe with high sensitivity and accuracy,and suitable for the determination of alkaloids and flavor compounds in cigarette,which was very important for the analysis of complex volatile trace substances in heated non-burning cigarette.

关 键 词：热脱附 冷阱 气相色谱-质谱联用 生物碱 香精 

分 类 号：O657.63[理学—分析化学] TS411[理学—化学]