Abstract: Components of volatile oil in petals of fresh peony were extracted by solid phase micro-extraction and analyzed by GC-MS, and their relative contents (in %) were found by the method of normalization. To attain a higher efficiency in SPME, the 50/30 μm PDMS/DVB/CAR fiber as coating was selected for the micro-extractor, the extraction was carried out at 45 ℃ for 40 min. Thirty-eight compounds were identified, and total mass fraction was amounting to 2 481.34 ng·g-1. The main compounds were found as following: hexyl acetate, citronellol, trans-geraniol and geranyl propionate, which were the important ingredients forming the fragrant characteristic of peony.