Chinese Journal of Chromatography

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Modification of mid-point restrictor of heart cut multidimensionalgas chromatography-mass spectrometry system and its application in analysis of benzo[a]pyrene in cigarette smoke

SHI Jiaqin*, LIU Baizhan, XIE Wenyan   

  1. Technical Center, Shanghai Tobacco (Group) Corporation, Shanghai 200082, China
  • Received:2009-11-26 Revised:2010-01-24 Online:2010-06-28 Published:1980-06-25
  • Contact: SHI Jiaqin

Abstract: The mid-point restrictor, known as the key spare part of multidimensional gas chromatography (MDGC), was modified and applied in the determination of benzo[a]pyrene in cigarette smoke. The graphite restrictor was replaced by a 0.25 mm i.d. fused silica open tubular and the two-hole graphite ferrule was replaced by a press-fit glass Y-splitter to improve the stability of retention time on the 1st dimensional column and eliminate the carry-over effects of graphite. The cigarette samples were prepared as follows: The mainstream cigarette smoke collected on Cambridge pad was extracted with cyclohexane, then the extractant was analyzed by heart cut MDGC-mass spectrometry(MS) directly with benzo[a]pyrene-d12 as internal standard. The method was proved to be simple, sensitive, fast and reliable with good linearity (linear range of 1.47-29.4 μg/L, r2 of 0.9999), reproducibility (relative standard deviation (RSD) of 1.94%), recovery (90.74%-101.86%) and low quantitative and qualitative detection limits. Moreover, the amount of benzo[a]pyrene in the 2R4F Kentucky reference cigarette smoke obtained by this method was close to that reported in literature.

Key words: benzo[a]pyrene, cigarette smoke , mass spectrometry (MS), multidimensional capillary gas chromatography (MDGC), mid-point restrictor