Analytical and Bioanalytical Chemistry

, Volume 409, Issue 11, pp 2993–3005 | Cite as

Simultaneous analysis of nine aromatic amines in mainstream cigarette smoke using online solid-phase extraction combined with liquid chromatography-tandem mass spectrometry

  • Jie Zhang
  • Ruoshi Bai
  • Zhaojuan Zhou
  • Xingyu Liu
  • Jun ZhouEmail author
Research Paper


A fully automated analytical method was developed and validated by this present study. The method was based on two-dimensional (2D) online solid-phase extraction liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) to determine nine aromatic amines (AAs) in mainstream smoke (MSS) simultaneously. As a part of validation process, AAs yields for 16 top-selling commercial cigarettes from China market were evaluated by the developed method under both Health Canada Intensive (HCI) and ISO machine smoking regimes. The gas phase of MSS was trapped by 25 mL 0.6 M hydrochloric acid solution, while the particulate phase was collected on a glass fiber filter. Then, the glass fiber pad was extracted with hydrochloric acid solution in an ultrasonic bath. The extract was analyzed with 2D online SPE-LC-MS/MS. In order to minimize the matrix effects of sample on each analyte, two cartridges with different extraction mechanisms were utilized to cleanup disturbances of different polarity, which were performed by the 2D SPE. A phenyl-hexyl analytical column was used to achieve a chromatographic separation. Under the optimized conditions, the isomers of p-toluidine, m-toluidine and o-toluidine, 3-aminobiphenyl and 4-aminobiphenyl, and 1-naphthylamine and 2-naphthylamine were baseline separated with good peak shapes for the first time. The limits of detection for nine AAs ranged from 0.03 to 0.24 ng cig−1. The recovery of the measurement of nine AAs was from 84.82 to 118.47%. The intra-day and inter-day precisions of nine AAs were less than 10 and 16%, respectively. Compared with ISO machine smoking regime, the AAs yields in MSS were 1.17 to 3.41 times higher under HCI machine smoking regime.

Graphical abstract

New method using online SPE-LC/MS/MS for analysis of aromatic amines in mainstream cigarette smoke


Online solid-phase extraction Liquid chromatography-tandem mass spectrometry Aromatic amines Mainstream cigarette smoke 



The authors thank Dr. Yongsheng Zhang (Zhengzhou University) for his helpful comments on the manuscript.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflicts of interest.

Supplementary material

216_2017_245_MOESM1_ESM.pdf (83 kb)
ESM 1 (PDF 82 kb)


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Copyright information

© Springer-Verlag Berlin Heidelberg 2017

Authors and Affiliations

  • Jie Zhang
    • 1
  • Ruoshi Bai
    • 1
  • Zhaojuan Zhou
    • 1
  • Xingyu Liu
    • 1
  • Jun Zhou
    • 1
    Email author
  1. 1.Beijing Third Class Tobacco Super vision StationBeijingChina

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