In this study, the feasibility of GC-MS was evaluated for the quantification of odorous volatile organic compounds (VOCs) in environmental samples. These included methyl ethyl ketone, isobutyl alcohol, methyl isobutyl ketone, and butyl acetate plus benzene, toluene, and xylene (BTX). For this purpose, the gaseous standard for these VOCs were analyzed by GC-MS with the aid of both direct injection (DI) into the GC injector and solid-phase microextraction (SPME). The liquid phase standard prepared independently was tested additionally by the DI method as a reference to gaseous calibration. The detection limit (DL) values, when tested for basic quality assurance in this study, showed large differences between DI (0.002-0.007 ng) and SPME method (1.03-1.81 ng) in terms of absolute mass. The DL values, when expressed in terms of concentration (v/v), showed considerable improvement in SPME (below 0.40 nmol mol(-1)) relative to the DI method (approximately 6-15 nmol mol(-1)). The reliability of the GC-MS method was further validated through an analysis of real environmental samples collected from an industrial area.