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The supercritical CO2 (SC-CO2) extraction process of black poplar (Populus nigra L.) buds was optimized (pressure, temperature) based on the yields of major phytochemicals (volatiles and non-volatiles). The optimal settings were 30MPa/60°C. Major volatiles determined by GC–MS in the optimized SC-CO2 extract (mg of benzyl salicylate equivalent (BSE) per 100g of buds) were: pinostrobin chalcone (1574.2), β-eudesmol (640.8), α-eudesmol (581.9), 2-methyl-2-butenyl-p-coumarate (289.9), pentyl-p-coumarate (457.0), γ-eudesmol (294.4), and benzyl salicylate (289.2). Partial qualitative similarity was observed between SC-CO2 extracts and corresponding hydrodistilled essential oil dominated by sesquiterpenes, but with lower yields. Major compounds (mg per 100g of buds) identified by UHPLC-DAD-QqTOF-MS in the optimized SC-CO2 extract were: pinostrobin (751.7), pinocembrin (485.6), 3-O-pinobanksin acetate and methyl-butenyl-p-coumarate (290.2; 144.9 of pinobanksin and p-coumaric acid equivalents, respectively). SC-CO2 extraction was found useful for green, efficient and simultaneous extraction of both volatile/non-volatile, bioactive phytochemicals of poplar buds – precursors of poplar-type propolis.Supercritical CO2 efficiently extracts volatiles and non-volatiles from poplar buds.The optimal supercritical CO2 extraction settings were 30MPa and 60°C.The obtained extracts are rich in bioactive sesquiterpenes and flavonoids.