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In this work, the sawmill waste from <i>Picea abies</i> debarking was considered as source of valuable phytoconstituents. The extraction was performed using different ethanol/water mixtures, and characterization was obtained by LC-MSⁿ. This latter revealed flavonoid glycosides, lignans, and procyanidins. Extraction with organic solvents (dichloromethane and methanol) and chromatographic separations of the obtained extracts by silica column followed by semi-preparative HPLC led to the isolation of polyphenols and terpenoids such as 21<i>α</i>-metoxy-serrat-14-en-3-one, 21<i>α</i>-hydroxy-serrat-14-en-3-one, pinoresinol, dehydroabietic acid, 15-hydroxy-dehydroabietic acid, 7-oxo-dehydroabietic acid, pimaric acid, 9<i>β</i>-pimara-7,15-dien-19-ol, 13-epi-manoyl oxide, taxifolin-3′-O-glucopyranoside, trans-astringin, and piceasides. Piceaside V and 9<i>β</i>-pimara-7-keto-19<i>β</i>-olide, two novel compounds identified for the first time in <i>P. abies</i> bark, were isolated, and their structures were elucidated using 1D and 2D NMR and MS techniques. The polyphenolic composition of the methanolic portion was also investigated using LC-MSⁿ, and the piceaside content was estimated. To assess the antioxidant activity of main constituents, semi-preparative HPLC was performed on the methanolic extract, and the obtained fractions were assayed by using the DPPH test. Overall, this work shows the potential usefulness of <i>P. abies</i> bark as a source of valuable phytochemicals.