In this study, the calibration characteristics of six new odorant VOCs along with two reference compound were evaluated based on GC-MS (SIM). For the proper evaluation of the GC/MS method, calibration of 7 VOCs were made both by the SPME and direct injection (DI). The minimum detection limit (MDL) of those VOC determined by SPME method fell in the range of 0.31∼0.38 ppb while those of DI from 6.18∼14.3 ppb. The analytical performance of our SPME/GC-MS method was compared against those tested previously by other study groups. Although more efforts are needed to establish the reliability of our SPME/GC-MS method, the method adapted in this study can be recommended as one of the standard methods for the analysis of the target VOCs in this study to settle formal experiment methods.