Abstract: The effects of inlet temperature, initial column temperature and column polarity on the determination of toluene diisocyanate content in adhesives by gas chromatography-mass spectrometry(GC-MS) were studied. The results showed that 200℃ inlet temperature, 100℃ initial column temperature and weak polar column or non-polar column were suitable for the analysis. Besides, the effect of water content in solvent on the test was investigated, indicating the importance of dewatering of reagent. Because most of the standards use FID detectors, the results of GC-MS were compared with those of GC-FID. It is found that the quantitative results of FID were basically consistent with those of MS. There for in practice, GC-MS can be used for the qualitative and quantitative analysis.