Abstract: 0.001 0 g of the nail sticker sample was placed into the 20 mL head-space flask, and the sampling of the 6 volatile organic compounds (VOCs, i.e., acetone, n-hexane, ethyl-acetate, iso-propyl acetate, toluene and butyl acetate) together with the treatment of solid phase microextraction (SPME) was carried out under the following optimized conditions:36℃ of incubation temperature, 15 min of incubation time, 300 r·min^-1 of rate of rotation of the vibrator, normal temperature of temperature for SPME and 10 times of frequency of extraction of sample. The VOCs (including the 6 compounds mentioned above) obtained in this process were then introduced into the instrument for GC-MS analysis. The chromatographic column of HP-VOC (60 m×0.25 mm, 0.25 μm) and the mode of programmed temperature elevation from 40℃ to 250℃ were adopted in the chromatographic separation, and conditions of EI and the mode of selective ionic scanning were applied in MS determinations. Outer standard method was used for quantification. Linear relationships between values of peak areas of the 6 VOCs and their respective masses were found in the same range of 2-250 ng, with their same detection limits (3.14s) of 0.5 ng. Using substantial samples as matrixes, recovery was tested by addition of mixed standards at 5 concentration levels, giving results of recovery in the range of 80.0%-110%. Values of RSDs (n=7) were found ranged from 0.030% to 5.0%.