▎ 摘　　要

Efficient fabrication of excellent fiber coatings for high-performance solid-phase microextraction (SPME) is interesting. Here, a high-efficiency synthesis strategy on graphene oxide/polyhedral oligomeric silsesquioxane (GO/POSS) composite-coated fiber was exploited via an ultra-fast UV polymerization in one step, and applied to excellent SPME of polycyclic musks (PCMs). Using methacryloxy siloxane-grafted GO and POSS-methacryl substituted (POSS-MA) as functional monomers, a facile and direct UV polymerization of multiple reactions including alkenyl radical reaction and thiol-ene click chemistry was fulfilled on thiol-pretreated fiber in only 5 min without tedious process. Characteristics such as morphology, FT-IR, XPS, BET and TG of fiber coating were studied in detail, as well as the SPME performance. Attributing to the rigid stereo conformation of POSS and large conjugate plane of GO-based nanosheet, the significant surface area, high hydrophobicity and intrinsic 7C-7C in-teractions were adopted in fiber coating. In comparison of commercial SPME fibers, POSS-based or GO-based SPME fibers, a superior extraction performance towards PCMs was achieved with GO/POSS-coated fiber. High-efficiency extraction of PCMs was gained with prominent enrichment factors and the sensitive detection limits of PCMs were of 0.04-0.12 ng/L. In particular, the extraction efficiency was robust and still maintained a high level above 93% for PCMs even after 150 cycle's applications. Good recoveries of PCMs reached 86.6%- 102.1% and 86.7%-101.3% in river water and cosmetic samples, respectively. It lights an attractive approach to efficiently fabricating robust GO/POSS-coated fiber for high-performance SPME of PCMs.