Abstract: An analytical method was developed for analyzing methyleugenol in mainstream cigarette smoke by using solid-phase extraction purification-double packing reverse extraction coupled with gas chromatography/mass spectrometry. The trapping method of target compound in mainstream smoke was studied, and the suitable solid-phase extraction condition was selected and optimized successively. By optimizing the amount of packings, a device with double packings was prepared for back extracting from water-organic solvent system. The influence on the chromatographic peak of target compound with different chromatographic injection mode was discussed, and the mass spectra ion parameters were finally decided. The results showed that: 1) under the optimized condition, the method presented good linear relationship (R²=0.999 5) in the range of 10-400 ng/mL. The intra-day and inter-day relative standard deviations (RSD) were 6.86% and 8.73% respectively, and the rate of spiked recovery was between 97.2% and 114.5%. The limit of detection (LOD) was 0.24 ng/cig, while the limit of quantization (LOQ) was 0.81 ng/cig, which were obviously better than the existing literature results. 2) By analyzing some cigarettes selected from the market, the yields of methyl eugenol in blended type cigarettes was in the range of 2.46-3.52 ng/cigarette, while 2.24-5.13 ng/cigarette in Virginia type cigarettes. In addition, the release amount of methyl eugenol per tar of the former was far higher than the latter.