Abstract: Volatiles compounds from twigs of Pinus massoniana were extracted by solid phase microextraction and steam distillation. Their constituents were analyzed by gas chromatography-mass spectrometry and compared. Twenty-six compounds were identified in the solid phase microextraction extracts, the main components were α-pinene, β-pinene, sabinene, isolongifolene and trans-caryophyllene. Thirty-nine compounds were identified in the steam distillation extracts, the major components were α-pinene, β-pinene, β-phellandrene, trans-caryophyllene, isolongifolene and camphene. The result showed that chemical compositions and relative contents of common compositions were different by means of different extracted methods.