Three kind of ASE (Accelerated Solvent Extraction) and SPMDs (Semi-Permeable Membrane Devices) combined methods (ASE-SPMDs, ASE-accelerated SPMDs and SPMDs without extraction) and general Soxhlet-GPC were compared each other for the analysis of PCDD/FS in sediment. The average recovery rate of three types ASE and SPMDs combined methods (108.1%) were higher than that of the Soxhlet-GPC (79.5%) for three samples in each method using surrogate internal standards. The average coefficient of variation (10%, $2.1{sim}25.2%$) for each congener of PCDD/Fs shows the reasonable results. Total PCDD/Fs concentrations after SPMDs without extraction were quite low, but those after ASE-SPMDs and ASE-accelerated SPMDs methods were close to the Soxhlet-GPC. Thus, the ASE-SPMDs and ASE-accelerated SPMDs methods are considered as the excellent pre-treatments method because they need less solvent and time without quality degradation.