Abstract: Organic compounds in toluene diisocyanate (TDI) polyurethane were extracted with acetone and were detected by gas chromatography-mass spectrometry (GC/MS) with capillary column. The quantitative analysis was performed by square peaks obtained with total ion chromatography to normalization. More than seventy peaks were separated, and 53 kinds of compounds were identified, their composition account for 94.48% of the total components. The TDI polyurethane was detected by pyrolysis chromatography-mass spectrometry, 35 kinds of compounds were identified. These data can be applied to the establishment of scientific basis for the detection of harmful chemistries in TDI polyurethane and the control of the products in quality.