A preparative gas chromatography (pGC) method was developed for the separation of volatile components from the methanol extract of Curcuma rhizome. The compounds were separated on a stainless steel column packed with 10% OV-101 (3 m × 6 mm, i.d.), and then, the effluent was split into two gas flows. One percent of the effluent passed to the flame ionization detector (FID) for detection and the remaining 99% were directed to the fraction collector. Five volatile compounds were collected from the methanol extract of Curcuma rhizome (5 g/mL) after 83 single injections (20 uL) with the yield of 5.1-46.2 mg. Furthermore, the structures of the obtained compounds were identified as β-elemene, curzerene, curzerenone, curcumenol, and curcumenone by MS and NMR spectra, respectively.