A multiresidue method based on normal-phase liquid chromatography (LC) cleanup and gas chromatography–electron capture detection–mass selective detection (GC–ECD–MSD) analysis has been developed for the determination of endosulfan and its main metabolic derivatives in human adipose tissues. Analytes were extracted by dissolving the fat samples in n-hexane, and the hexanic extracts were directly injected onto the silicagel column of the automated LC cleanup system. Purified LC extracts were analyzed by GC–ECD or GC–MSD, without any solvent exchanges or pre-concentration steps. The high efficiency of the high-performance liquid chromatographic cleanup for the elimination of fats allowed to reach detection limits for all analytes at low nanograms-per-gram concentration levels. The optimized overall analytical procedure was applied to 18 selected human mammary adipose and abdominal fat tissue samples. p,p'-DDE, hexachlorobenzene, and b-HCH were the most frequently detected compounds, and residues of endosulfan-sulfate and -ether were also found in several samples. All findings were confirmed by an additional GC–MS–MS analysis of the LC sample extracts.