Abstract: A supercritical fluid extraction cell filled with adsorbent (Carbotrap and Carbotrap C) was used directly as a sampling tube to adsorb volatile organic peroxides in gas phase and liquid phase respectively.And then they were extracted by supercritical fluid CO2 with methanol as a modifier.The experimental results showed that under the relatively low temperature(35 ℃) and high pressure(40 MPa)the recoveries of nonpolar and lowpole organic peroxides were high enough to meet the demand for the quantitative analysis.No visible decomposition of organic peroxides was found during the supercritical fluid extraction.It is a good method to enrich thermally unstable compounds using SFE technique as long as lower temperature was controlled during the extraction process.