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

引用本文: 陈凤明, 张峰, 高飞, 雍炜, 杨敏莉, 冯峰. 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[J]. 分析化学, 2021, 49(1): 128-136. doi: 10.19756/j.issn.0253-3820.201555 shu

Citation: CHEN Feng-Ming, ZHANG Feng, GAO Fei, YONG Wei, YANG Min-Li, FENG Feng. 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[J]. Chinese Journal of Analytical Chemistry, 2021, 49(1): 128-136. doi: 10.19756/j.issn.0253-3820.201555 shu

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

中国检验检疫科学研究院, 北京 100176

通讯作者: 张峰,E-mail:fengzhang@126.com

基金项目:
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1~500 μg/L，线性相关系数（R²）均大于0.993，方法检出限为0.02~0.50 μg/kg，定量限为0.10~2.0 μg/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。

关键词:

English

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

Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China

Corresponding author: ZHANG Feng, fengzhang@126.com

Received Date: 14 September 2020
Revised Date: 03 November 2020
Fund Project:
Supported by the Central Public-Interest Scientific Institution Basal Research Fund (No.2018JK001).

Abstract: 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 1-500 μg/L, the linear correlation coefficient (R²) was greater than 0.993, and the limits of detection (LOD) and limits of quantitation (LOQ) were 0.02-0.50 μg/kg and 0.1-2.0 μg/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.

Key words:

1. [1]
  YIN F, ZHANG X M, SONG S Q, HAN T, ERIC K. Eur. Food. Res. Technol., 2016, 242(6):869-880.
2. [2]
  HE Q, ZHANG Y P, ZHOU S, SHE S K, CHEN G, CHEN K B, YAN Z J, GUO D F. Flavour Frag. J., 2015, 30(3):230-237.
3. [3]
  LI Ang-Ze, WANG Xian-Shuang, XU Xiang-Jun, HE Ya-Ge, GUO Shuai, LIU Yu-Fei, GUO Wei, LIU Rui-Bin. Chin. Opt., 2019, 12(5):1139-1146. 李昂泽, 王宪双, 徐向君, 何雅格, 郭帅, 柳宇飞, 郭伟, 刘瑞斌. 中国光学, 2019, 12(5):1139-1146.
4. [4]
  XIE Xiao-Tian, ZHENG Ping, ZHU Wei-Ming. Chin. J. Anal. Chem., 2000, 28(9):1085-1087. 谢笑天, 郑萍, 朱伟明. 分析化学, 2000, 28(9):1085-1087.
5. [5]
  ZHOU Ze-Hong, CAO Lin-Hai, WANG Chang-Quan, LI Qi-Quan, LI Bing, LI Shan. Chin. Tobacco Sci., 2016, 37(2):65-70. 周泽弘, 曹淋海, 王昌全, 李启权, 李冰, 李珊. 中国烟草科学, 2016, 37(2):65-70.
6. [6]
  DENG Xiao-Hua, ZHOU Qing-Ming, ZHOU Ji-Heng, LI Juan. Acta Tabacaria Sin., 2011, 17(3):17-22. 邓小华, 周清明, 周冀衡, 黎娟. 中国烟草学报, 2011, 17(3):17-22.
7. [7]
  WANG P, DAI Y, ZHOU X Z, CHENG K Y, XIAO K Y, MA K Y, LI H L, DU H Y, ZHANG Y, WANG C G. Tobacco Sci. Technol., 2017, 50(13):43-49.
8. [8]
  LIU Chun-Kui, LIU Yan-Fang, LIU Hui-Jie, YAN Qi-Feng, JIA Lin, MA Ming, MA Lin, XIA Yang, YU Dong-Ming, ZHANG Xiao-Fei, LI Qing-Xiang, ZHANG Jun-Song. J. Southern Agric., 2019, 50(6):1319-1327. 刘春奎, 刘艳芳, 刘会杰, 闫启峰, 贾琳, 马明, 马林, 夏阳, 誉东明, 张晓飞, 李庆祥, 张峻松. 南方农业学报, 2019, 50(6):1319-1327.
9. [9]
  MIRANDA A B, MARTÌNEZ C P, CHACÕN J J, PRIETO M A. J. Near Infrared Spec., 2019, 27(2):123-133.
10. [10]
  YU Jie, XIONG Jun-Wei, SHA Yun-Fei, YUE Bao-Hua, GE Jiong. J. Univ. Jinan, 2019, 33(2):150-155. 于洁, 熊骏威, 沙云飞, 岳宝华, 葛炯. 济南大学学报, 2019, 33(2):150-155.
11. [11]
  LI Hao-Hao, LI Wei, ZHAO Shi-Min, JIANG Kai, LI Zhao-Min, LIU Meng-Meng, ZHU Tao-Yue. J. Anhui Agric. Sci., 2014, 42(29):10318-10321. 李豪豪, 李威, 赵世民, 江凯, 李照民, 刘萌萌, 朱桃月. 安徽农业科学, 2014, 42(29):10318-10321.
12. [12]
  CHEN Sen-Lin, HUANG Man-Yan, LIN Yun, TAO Hong, HU Yu-Ling, YE Wei-Min, LI Gong-Ke. Chin. J. Anal. Chem., 2019, 47(5):725-730. 陈森林, 黄曼艳, 林云, 陶红, 胡玉玲, 叶为民, 李攻科. 分析化学, 2019, 47(5):725-730.
13. [13]
  LOCHMANM H, BAZZANELLA A, KROPSCH S, BACHMANN K. J. Chromatogr. A, 2001, 917:311-317.
14. [14]
  XU Qing-Ping, HE You-Zhao. Chin. J. Chromatogr., 2006, 24(4):392-395. 许庆平, 何友昭. 色谱, 2006, 24(4):392-395.
15. [15]
  SCHWANZ T G, BOKOWSKI L V V, MARCELO M C A, JANDREY A C, DIAS J C, MAXIMIANO D H, CANOVA L S, PONTES O F S, SABINA G P. Talanta, 2019, 202:74-89.
16. [16]
  ZHANG Feng-Mei, JIANG Wei, LIU Chun-Bo, SHEN Qin-Peng, SI Xiao-Xi, ZHU Rui-Zhi, TANG Shi-Yun, HE Pei, LI Zhen-Jie, LIU Zhi-Hua. Tobacco Sci. Technol., 2018, 51(7):46-53. 张凤梅, 蒋薇, 刘春波, 申钦鹏, 司晓喜, 朱瑞芝, 唐石云, 何沛, 李振杰, 刘志华. 烟草科技, 2018, 51(7):46-53.
17. [17]
  CUI Ting-Hui, LI Heng, TANG Shi-Yun, LIU Chun-Bo, GAO Xiao-Hua, LI Zhen-Jie, ZHANG Feng-Mei, YANG Guang-Yu, JIANG Wei, LIU Zhi-Hua, MIAO Ming-Ming, HE Pei, SHEN Qin-Peng. J. Instrum. Anal., 2018, 37(7):766-771. 崔婷惠, 李恒, 唐石云, 刘春波, 高晓华, 李振杰, 张凤梅, 杨光宇, 蒋薇, 刘志华, 缪明明, 何沛, 申钦鹏. 分析测试学报, 2018, 37(7):766-771.
18. [18]
  MA Li-Chao, XIAO Xiao-Ming, LI Deng-Ke, XING Li-Xia, ZHANG Chun-Tao. Chin. J. Anal. Lab., 2016, 25(2):228-232. 马立超, 肖晓明, 李登科, 邢立霞, 张春涛. 分析试验室, 2016, 25(2):228-232.
19. [19]
  ABDALLAH I A, HAMMELL D C, STINCHCOMB A L, HASSAN H E. J. Chromatogr. B, 2016, 1020:67-77.
20. [20]
  FAMEL M, PALMISANIi J, FERRANITI C, ABENAVOLI C, PALLESCHI L, MANCINELLI R, FIDENTE R M, GENNARO G, DRAISCI R. J. Sep. Sci. 2017, 40:1049-1056.
21. [21]
  HU R S, WANG J, LI H, NI H, CHEN Y F, ZHANG Y W, XIANG S P, LI H H. Sep. Purif. Technol., 2015, 146:1-7.
22. [22]
  WEYMARN L B, THOMSON N M, DONNYE C, HATSUKAMI D K, MURPHY S E. Chem. Res. Toxicol, 2016, 29:390-397.
23. [23]
  ZHAO G H, YU Y L, ZHOU X T, LU B Y, Li Z M, FENG Y J. Waste Manage. Res., 2017, 35(5):534-540.
24. [24]
  LUO Yan-Bo, CHEN Xiao-Jing, LI Xiang-Yu, ZHANG Hong-Fei, ZHU Feng-Peng, JIANG Xing-Yi, PANG Yong-Qiang. Chin. J. Anal. Chem., 2020, 48(6):794-801. 罗彦波, 陈小静, 李翔宇, 张洪非, 朱风鹏, 姜兴益, 庞永强, 分析化学, 2020, 48(6):794-801.
25. [25]
  ZHOU Peng, HONG Yi, ZHANG Qi, HUANG Bao, ZHU Hui, MO Ting, HUANG Zheng-Xu. J. Instrum. Anal., 2019, 38(9):1079-1084. 周鹏, 洪义, 张祺, 黄保, 朱辉, 莫婷, 黄正旭. 分析测试学报, 2019, 38(9), 1079-1084.
26. [26]
  CAMPBELL C G, ASTORGA D J, CELINA M. Polym. Degrada. Stab., 2020, 174:109032.
27. [27]
  CUI Yang, LI Xue-Mei, YANG Ye-Kun, ZENG Xiao-Ying, ZHE Wei, DUN Yan-Qing, LI Gan-Peng. Chin. J. Anal. Chem., 2010, 38(2):275-279. 崔杨, 李雪梅, 杨叶昆, 曾晓鹰, 者为, 段焰青, 李干鹏. 分析化学, 2010, 38(2):275-279.

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沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 张峰,E-mail:fengzhang@126.com

English

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

Corresponding author: ZHANG Feng, fengzhang@126.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 张峰,E-mail:fengzhang@126.com

English

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

Corresponding author: ZHANG Feng, fengzhang@126.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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