Abstract: GC-MS/MS with headspace-solid phase micro-extraction (HS-SPME) was applied to the determination of safrole in essence and perfume. To attain a higher efficiency in SPME, 65 μm PDMS/DVB fiber was selected as coating for the micro-extraction, and the extraction was carried out at (25±5) ℃ for 30 min. The analyte were separated on DB-5MS capillary column and detected by EI ion source with MS/MS. The ions with m/z of 162 and 131 were selected as parent ion and daughter ion respectively for safrole, and the ion with m/z 104 was selected as quantitative ion for the internal standard of phenylethyl propionate. Linearity range for safrole was between 20-1 000 ng·g-1, with detection limit (3S/N) of 2.2 ng·g-1. Tests for recovery were performed by addition of standard of safrole at 3 concentration levels for 5 parallel determinations each, results of average recovery found were in the range of 71.1%-114.3% with RSD′s (n=5) in the range of 3.4%-16%.