Abstract: Two portions of the powdered walnut shell sample were extracted separately by Soxhlet′s extraction with mixed solvent of CH2Cl2-CH3OH (93+7), and by reflux-extraction with mixed solvent of CH2Cl2-CH3OH-H2O (93+7+100) under heating. The extracts obtained were determined separately by GC-MS. In the extract obtained by Soxhlet′s extraction 34 chemical components were identified and determined and in the extract obtained by reflux extraction 13 chemical components were identified and determined. The main compounds in the extract obtained by the two methods were the following: organic acids, esters of organic acids, aldehydes, phenols, alcohols, ketones and naphthalenes, etc..