Abstract: Shenmu char powder (SCP) was sequentially extracted with petroleum ether, carbon disulfide, dichloromethane, acetone, and methanol in a Soxhlet extractor to obtain extracts 1-5 (E_1-5) and final residue. The total extract yield of SCP is 1.76%. All the extracts were characterized with gas chromatograph/mass spectrometer (GC/MS), atmospheric solid analysis probe/time-of-flight mass spectrometer (ASAP/TOF-MS), and electrospray ionization/time-of-flight mass spectrometer (ESI/TOF-MS). Normal alkanes with C₁₅ to C₂₄ and arenes with 3 and 4 rings are predominant in E₁ and E₂, respectively, while more heteroatom-containing organic species were identified in E_3-5. Organooxygen compounds are the most abundant in E₄ and E₅ based on analysis with GC/MS. Much more heteroatom-containing organic compounds were detected in E_3-5 with ASAP/TOF-MS and ESI/TOF-MS than with GC/MS.