Abstract: GC with single dropping microextraction was applied to the determination of 4 anilines, i.e., aniline, N, N-dimethyl aniline, o-toluidine and m-toluidine in water. Analytical conditions were studied and the following optimized parameters were given: ① extractant: n-hexane; ② temperature of extraction: 25 ℃; ③ height of droplet from surface of liquid in extraction bottle: 2.0 cm; ④ time of extraction: 13 min; ⑤ rate of stirring: 400 r·min-1. Linear relationships between values of mass concentration and peak area of the 4 anilines were kept in the same range of 0.100-1.00 μg·L-1 with limits of detection in the range of 0.006-0.014 μg·L-1. The proposed method was used in the analysis of water sample, giving values of recovery obtained by standard addition method in the range of 90.0%-115% and values of RSD′s (n=6) less than 10%.