Citation: SHEN Qin-Peng, LIU Qiang, XIANG Neng-Jun, LIU Chun-Bo, HE Pei, LIU Zhi-Hua, YANG Guang-Yu, YOU Jun-Heng, MIAO Ming-Ming. Online Liquid Chromatography-Gas Chromatography-Mass Spectrometry for Highly Sensitive Determination of 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanone in Mainstream Cigarette Smoke[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(6): 929-934. doi: 10.11895/j.issn.0253-3820.150876 shu

Online Liquid Chromatography-Gas Chromatography-Mass Spectrometry for Highly Sensitive Determination of 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanone in Mainstream Cigarette Smoke

Key Laboratory of Tobacco Chemistry of Yunnan Province, Research and Development of Center, China Tobacco Yunnan Industrial Co., Ltd., Kunming 650231, China

Received Date: 2 November 2015
Revised Date: 12 January 2016

Fund Project: This work was supported by the National Natural Science Foundation of China (No.21365026)

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A new approach based on online coupled liquid chromatography-gas chromatography-mass spectrometry (LC-GC/MS) was developed for the rapid determination of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK) in mainstream cigarette smoke, in which a switching valve was employed to online switching between two-dimensional chromatography. The online LC-GC/MS system used in this study was built by using online gel permeation chromatography-gas chromatography-mass spectrometry except that the micro gel column was replaced by micro alkaline alumina column which was prepared by ourselves before. The NNK in mainstream cigarette smoke was collected by a Cambridge filter pad, then the pad was extracted with dichloromethane, and the extract was quantitatively analyzed by online LC-GC/MS with D4-NNK as an internal standard. Online LC-GC/MS allowed online pretreatment purification, and the sample was subjected to online LC-GC/MS without any prior purification, which reduced human error in analysis process. The injection volume of the present online LC-GC/MS could reach 40 μL, which was 20 times of that of the conventional GC/MS (2.0 μL of injection volume), and thus significantly improved the sensitivity. Under the optimum conditions, good linearity (r=0.9998) was obtained over the range of 1.2-120 ng/mL. The recoveries at three spiked levels ranged from 93.9% to 96.0%, and the limits of detection for qualitative and quantitative detection were 0.25 ng/mL and 0.9 ng/mL, respectively. All the results obtained by the present method are comparable to those of standard method recommend by China National Tobacco Company.
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