A novel analytical method, using gas chromatography-electron capture detection (GC-ECD) and GC-mass spectrometry detection (MS), was developed for the qualitative and quantitative measurement of pentachlorophenol in meat and fish. The analyte was extracted by methanol-2% trichloroacetic acid (3/1, v/v) with accelerated solvent extraction (ASE). The eluted fraction was evaporated and derivatized with acetic anhydride-pyridine (1/1, v/v) for GC-ECD analysis and GC-MS confirmation. The parameters for extraction pressure, temperature and cycle of ASE, cleanup, derivatization and analysis procedure were optimized. The averaged decision limits and detection capability of the method were in the ranges of 0.25-0.41 and 0.49-1.01 µg/kg in the muscle and liver of swine and bovine and in the muscle of carp and finless eel, respectively. Spiked recoveries from levels of 0.5-2.0 µg/kg were found to be more than 71.1%, with relative standard deviation less than 14.7% in GC-ECD and GC-MS. This rapid and reliable method can be used for the characterization and quantification of residues of pentachlorophenol in animal and fish tissues.