Aerial parts of Daphne pontica were collected from Ilgaz-cankiri, and D. oleoides subsp. oleoides was collected from 2 different localities (Ayranci-Karaman and Ilgaz-Cankiri) in Turkey. The samples were subjected to hydrodistillation and microdistillation. The resulting volatile samples were analyzed both by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS), respectively. The main components for D. pontica were identified as hexahydrofarnesyl acetone (8.6%), carvacrol (8.5%), dihydroedulane 11 (4.7%), (E)-geranyl acetone (4.6%), and thymol (4.5%), while nonacosane (42.5% and 27.2%), hexadecanoic acid (24.4% and 20.0%), phytol (12.3%), and carvacrol (5.0%) were identified as the main components of D. oleoides subsp. oleoides obtained by hydrodistillation. Carvacrol (12.0%), thymol (7.7%), dihydroactinidiolide (7.2%), bicydosesquiphellandrene (5.5%), and (Z)-3-hexenal (4.1%) were the major components in D. pontica, while carvacrol (27.2% and 25.4%), nonacosane (24.6%), (Z)-3-hexenal (18.5% and 2.5%), decane (7.4%), hexahydrofarnesyl acetone (7.4% and 2.2%), hexanal (6.6% and 1.5%), heptacosane (6.1%), nonanal (5.6% and 1.9%), thymol (5.1% and 2.3%), and phytol (5.0%) were identified in the D. oleoides subsp. oleoides isolated by microdistillation, respectively. In addition, the volatile components were evaluated for their ability to scavenge 1,1-dipheny1-2-picrylhydrazyl (DPPH) radicals using a bioautographic thin layer chromatography (TLC) method, and the samples showed activity comparable with that of the tested standards, vitamins C and E.