Abstract: GC-MS was applied to the determination of 24 harmful substances in shoe adhesives. The sample (0.200 0-0.500 0 g) was extracted ultrasonically for 60 min with ethyl acetate, and the extract was made up its volume to 50 mL with ethyl acetate, and filtered through organic phase microporous membrane of 0.45 μm. VF-624MS chromatographic column was used for GC separation, full-scanning mode and selected ion monitoring mode were adopted in MS analysis, and external standard method was used for quantification. Linear relationships between values of peak areas and mass concentrations of 24 harmful substances were found in definite ranges, with values of detection limits (3S/N) in the range of 0.02-0.10 g·kg^-1. Test for recovery was made by standard addition at 3 concentration levels, giving results in the range of 85.9%-116%, with RSDs (n=6) all less than 6.0%.