Abstract: A novel device, termed as gas purge microsyringe extraction (GP-MSE), has been developed and applied to the preparation of different kinds of oil samples, including condensates, light and normal oils for the first time.Oils from the Pearl River Mouth Basin were firstly extracted by GP-MSE and then qualitatively and quantitatively analyzed by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS).The proposed method has many advantages over traditional column chromatography, such as simple and fast steps, satisfactory recoveries, and lower consumption of solvents and samples.The relative standard deviations (RSD%) of adamantane and diamantane are 1.57% and 2.63%, respectively.Crude oil samples are purified and enriched effectively. The relative deviation is less than 9%, and the correlation coefficient is over 0.997.