Abstract: The cosmetic sample (1.000 g) was dissolved ultrasonically in dimethylsulfoxide (DMSO) and made up to 50 mL with the same solvent. An aliquot of 5.00 mL of the sample solution was introduced into the head-space flask and equilibrated at 85 ℃ for 30 min. The volatile organic compounds (VOC) were separated by passing through the HP-5MS quartz capillary column under the mode of programed temperature elevation from 50 ℃ to 220 ℃. Ionization source of EI and SIM mode of detection were adopted in MS determinations. Linear relationships between values of peak areas and mass concentrations of the 14 VOC′s were found in the same range of 0.001-1.0 mg·L-1, and values of DL′s (3S/N) for the 14 VOC′s found were range from 0.019 to 0.068 μg·g-1. Test for recovery was made by standard addition method at the concentration levels of 1.0, 20.0 mg·kg-1 using 2 substantial cosmetic samples as matrixes, giving results of recovery in the range from 82.1% to 112%, with values of RSD′s (n=6) all less than 5.0%.