Abstract: In order to synchronously detect five T&O compounds, this study applied automation headspace solid phase micro extraction - gas chromatography- mass spectrometry as the optimized conditions as follows: extraction sample volume of 10 mL, extraction temperature and time of 65 ℃ and 30 min respectively with preheating time of 5 min and desorption time of 2 min prior to the analysis. The method exhibited high sensitivity with the detection limit lowered as 1.5 ng/L, and high linearity (regression coefficients R² > 0.98) when the concentrations ranged within 1 to 1000 ng/L. The automatic solid phase micro extraction mode significantly reduced the complexity of traditional extraction methods. The attained method was applied to test the T&O compounds-producing algae, the results showed that the concentration of 2-MIB and β-Ionone were as high as 136.78 g/L and 1347.88 ng/L respectively when cell density reached 300 million/L, indicating that this method was reliable to analyze the T&O compounds in samples with complex background.