(NPs) with a large surface area and employed it as a novel fiber coating for extracting and determining volatile compounds from Ziziphora tenuior in a minimum period of time without using solvents with head solid-phase microextraction. The simplex approach was applied to optimize all parameters concurrently. Major optimized parameters include temperature, extraction time, and sample weight. In optimal circumstances, the repeatability for one fiber (n=5) was at the range of 2.8 – 9.2 percent for the sample compounds, which is given as relative standard division (R.S.D. %). The approach suggested in this work provides advantages such as simple usage, short analysis time, cheaper equipment, high relative recovery, and fiber thermal stability compared to common analysis approaches. Our findings indicated that γ-Fe2O3@SiO2-PW fibers are appropriate for the HS-SPME analysis of essential oils.