Acorus macrospadiceus is a common medicinal and food plant used different ethnic groups in Guizhou and surrounding areas. In this paper, the leaf and rhizome tissues of A. macrospadiceus were hydro-distilled to extract the volatile oils. The chemical constituents of these oils were analyzed by GC-MS and identified using the NIST 14.0 & NIST 14.0s mass spectral libraries. The relative contents of chemical constituents from the different plant parts were determined by area normalization. The analysis of A. macrospadiceus volatile oils resulted in the identification of 25 compounds from the leaf and 36 compounds from the rhizome. The identified compounds accounted for 97.85% of the leaf essential oil content and 97.18% of the rhizome essential oil content. The main volatile constituent of A. macrospadiceus was identified as estragole (93.56% of total oil content in leaf and 71.62% of total oil content in rhizome). Fourteen compounds were found to be common to essential oils of both leaf and rhizome. However, the relative amounts of these compounds were significantly different between the plant parts; the remaining identified compounds were unique to each part. This comparison of volatile oils from the different parts of A. macrospadiceus can serve as a reference for future development. Because of the higher estragole content and better harvesting sustainability of the leaves compared to rhizomes, the leaves of A. macrospadiceus deserve consideration for sustainable development. However, when we use it as a medical plant, we should draw a distinction between it with A. tatarinowii.