The brown alga Pelvetia canaliculata is one of the species successfully adapted to intertidal conditions. Inhabiting the high intertidal zone, Pelvetia spends most of its life exposed to air, where it is subjected to desiccation, light, and temperature stresses. However, the physiological and biochemical mechanisms allowing this alga to tolerate such extreme conditions are still largely unknown. The objective of our study is to compare the biochemical composition of Pelvetia during the different phases of the tidal cycle. To our knowledge, this study is the first attempt to draft a detailed biochemical network underneath the complex physiological processes, conferring the successful survival of this organism in the harsh conditions of the high intertidal zone of the polar seas. We considered the tide-induced changes in relative water content, stress markers, titratable acidity, pigment, and phlorotannin content, as well as the low molecular weight metabolite profiles (GC-MS-based approach) in Pelvetia thalli. Thallus desiccation was not accompanied by considerable increase in reactive oxygen species content. Metabolic adjustment of P. canaliculata to emersion included accumulation of soluble carbohydrates, various phenolic compounds, including intracellular phlorotannins, and fatty acids. Changes in titratable acidity accompanied by the oscillations of citric acid content imply that some processes related to the crassulacean acid metabolism (CAM) may be involved in Pelvetia adaptation to the tidal cycle.