Abstract: Phenol in mainstream of cigarette smoke was trapped in 35 mL of dilute acetic acid solution (1+99 by vol.).The solution obtained was diluted to 50 mL,from which an aliquot of 2.0 mL was taken for the rapid HPLC analysis.The ZORBAX Stable Bound column (2.1 mm×50 mm,1.8 μm) was used for the rapid separation,and mixtures of acetonitrile (containing 1% by volume of acetic acid) and dil.acetic acid solution (1+99) mixed in various ratios were used as mobile phase in the gradient elution.Fluorescence detection with the wavelengths of 272 nm (λex) and 310 nm (λem) was adopted in the determination.Only 5.0 min were required for a determination.The repeatability and reproducibility of the method were tested,giving values of RSD′s (n=7) 2.8% and 4.6% respectively.Test for recovery was made by standard addition method at 3 concentration levels,values of recovery found were in the range of 95%-103%.