Abstract:The methanol extract of the aerial parts of the medicinal plant Pedicularis sibthorpii Boiss., Scrophulariaceae, growing in the Azerbaijan province of Iran, was found to be active in the 2,2-diphenyl-1-picryl-hydrazyl (DPPH) and the antibacterial agar well diffusion assays, but no general toxicity was observed in the brine shrimp lethality assay. A combination of solid-phase extraction (SPE) and preparative reversed-phase high-performance liquid chromatography (prep-RP-HPLC) analyses of the methanolic extract afforded three phenylethanoids (verbascoside, martynoside and isomartynoside), an iridoid (aucubin), a flavonoid (luteolin 7-O-β-D-glucopyranoside) and mannitol, and the structures of these compounds were elucidated unambiguously by spectroscopic means. The distribution of the isolated compounds within the genus Pedicularis has also been discussed.