色谱

色谱 ›› 2017, Vol. 35 ›› Issue (10): 1105-1110.DOI: 10.3724/SP.J.1123.2017.06020

• 技术与应用 • 上一篇    

气相色谱-串联质谱法同时测定卷烟滤嘴中15种多环芳烃

张小涛1,2, 张丽1, 阮艺斌1, 王维维1, 姬厚伟1, 万强1, 林福呈2, 刘剑1   

  1. 1. 贵州中烟工业有限责任公司技术中心, 贵州 贵阳 550009;
    2. 浙江大学农业与生物技术学院, 浙江 杭州 310058
  • 收稿日期:2017-06-21 出版日期:2017-10-08 发布日期:2017-10-18
  • 通讯作者: 刘剑,Tel:(0851)83981463,E-mail:jliuemail@163.com.
  • 基金资助:

    贵州中烟工业有限责任公司科技项目（GZZY/KJ/JS/2016CW026-0）.

Simultaneous determination of 15 polycyclic aromatic hydrocarbons in cigarette filter by gas chromatography-tandem mass spectrometry

ZHANG Xiaotao1,2, ZHANG Li1, RUAN Yibin1, WANG Weiwei1, JI Houwei1, WAN Qiang1, LIN Fucheng2, LIU Jian1   

  1. 1. Technology Center, China Tobacco Guizhou Industrial Co. Ltd., Guiyang 550009, China;
    2. College of Agriculture & Biotechnology, Zhejiang University, Hangzhou 310058, China
  • Received:2017-06-21 Online:2017-10-08 Published:2017-10-18
  • Supported by:

    Science and Technology Project of China Tobacco Guizhou Industrial Co., Ltd. (No. GZZY/KJ/JS/2016CW026-0).

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摘要：

建立了气相色谱-串联质谱同时检测卷烟滤嘴中15种多环芳烃的方法。卷烟滤嘴用二氯甲烷振荡萃取后，经0.22 μm有机相滤膜过滤，采用DB-5MS色谱柱（30 m×0.25 mm， 0.25 μm）进行分离，电子轰击源、正离子模式下以多反应监测模式进行检测，内标法进行定量。15种多环芳烃（苊烯、苊、芴、菲、蒽、荧蒽、芘、苯并［a］蒽、屈、苯并［b］荧蒽、苯并［k］荧蒽、苯并［a］芘、二苯并［a，h］蒽、苯并［g，h，i］苝和茚并［1，2，3-c，d］芘）的线性关系良好，相关系数（R2）为0.9914~0.9999。15种多环芳烃在低、中、高3个添加水平下的平均回收率为81.6%~111.2%；除了芴在低添加水平时相对标准偏差为19.2%外，其他相对标准偏差均小于16%。15种多环芳烃的检出限为0.02~0.24 ng/滤嘴，定量限为0.04~0.80 ng/滤嘴。方法前处理简便，具有快速、准确、灵敏度高及重复性好的优点，适用于卷烟滤嘴中多环芳烃的分析。

关键词: 多环芳烃, 卷烟, 滤嘴, 气相色谱-串联质谱

Abstract:

A method for the simultaneous determination of 15 polycyclic aromatic hydrocarbons in cigarette filter was developed by isotope internal standard combined with gas chromatography-tandem mass spectrometry. The cigarette filters were extracted with dichloromethane, and the extract was filtered with 0.22 μm organic phase membrane. The samples were isolated by DB-5MS column (30 m×0.25 mm, 0.25 μm) and detected using multiple reaction monitoring mode of electron impact source under positive ion mode. The linearities of the 15 polycyclic aromatic hydrocarbons (acenapthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, ben[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenzo[a,h]anthracene, benzo[g,h,i]perylene and indeno[1,2,3-c,d]pyrene) were good, and the correlation coefficients (R2) ranged from 0.9914 to 0.9999. The average recoveries of the 15 polycyclic aromatic hydrocarbons were 81.6%-109.6% at low, middle and high spiked levels, and the relative standard deviations were less than 16%, except that the relative standard deviation of fluorene at the low spiked level was 19.2%. The limits of detection of the 15 polycyclic aromatic hydrocarbons were 0.02 to 0.24 ng/filter, and the limits of quantification were 0.04 to 0.80 ng/filter. The method is simple, rapid, accurate, sensitive and reproducible. It is suitable for the quantitative analysis of the 15 polycyclic aromatic hydrocarbons in cigarette filters.

Key words: cigarette, filter, gas chromatography-tandem mass spectrometry (GC-MS/MS), polycyclic aromatic hydrocarbons (PAHs)

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