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) to charaterize agarwood incense. The work involved three types of SPME fibres at 30 minutes sampling time. The fibres are 50/30 µm divinylbenzene-carboxenpolydimethysiloxane (DVB-CAR-PDMS), 65 µm polydi methylsiloxanedivinylbenzene (PDMS-DVB) and 85 µm carboxen-polydimethyl siloxane (CAR-PDMS). The results showed that among many compounds extracted by GC-MS coupled with SPME, six compounds were found significantly presence in high quality aganvood incense due to their high percentage area (%). They are beta-maaliene, alpha-elemol, beta-selinene, 10-epi-gamma-eudesmol, agarospirol and caryophellene oxide. The finding offers a new approach for establishing the volatile profile of agarwood incense components which is beneficial for agarwood grading and discrimination.