This paper presents the application of Solid Phase Micro Extraction (SPME) coupled with Gas Chromatography - Mass Spectrometry (GC-MS) and Gas Chromatography - Flame Ionization Detector (GC-FID) in characterizing the agarwood incense. The work involved three types of SPME fibres at 30 minute sampling time. The fibres are 50/30 μm divinylbenzene-carboxen-polydimethysiloxane (DVB-CAR-PDMS), 65 μm polydi methylsiloxane-divinylbenzene (PDMS-DVB) and 85 μm carboxen-polydimethyl siloxane (CAR-PDMS). The results showed that among the many compounds extracted by GC-MS coupled with SPME, six compounds were substantially found in high quality agarwood incense due to their high percentage area (%). They are β-maaliene, α-elemol, β-selinene, 10-epi-γ-eudesmol, agarospirol and caryophellene oxide. The finding offers a new approach for establishing the volatile profile of agarwood incense components as well as for agarwood grading and discrimination.