The characteristic disagreeable odor of the stipes of Coprinus picaceus was very similar to the well-known skatole odor. Hence, this study checked the mushroom for volatile indoles and found skatole and traces of indole to be present not only in the stipes but also in the less odorous caps. A rapid enrichment procedure using a C-18 silica gel cartridge was employed to avoid substantial losses of apolar indoles (since conventional solvent/solvent extraction often led to such losses). Fruit bodies were collected, minced, homogenized, and the supernatant was passed through a pre-equilibrated C-18 cartridge; adsorbed substances were eluted with dichloromethane/1% methanol. GC/MS (Varian MAT 311 A mass spectrometer) and TLC (silica gel plates, van Urk reagent) analyses were performed. Results showed skatole (96% of total amount) as the major component and indole (4% of total amount) as a trace component. GC/MS fragments of skatole matched literature data, and TLC behavior was identical to authentic compounds. This study demonstrates that skatole is the major component of the odor in C. picaceus stipes, and our GC/MS and TLC analysis revealed that the disagreeable odor of C. picaceus is due to skatole as the main component. This is the first description of skatole being a constituent of a mushroom verified by GC/MS analysis.