The aim of this study was to provide chemical characterization of unexplored macroalgae from the Adriatic Sea; brown alga Fucus virsoides, red alga Amphiroa rigida and green alga Codium bursa. Various methods were used to determine the volatilome profiles of fresh, air-dried and freeze-dried samples, including headspace solid-phase microextraction (HS-SPME), hydrodistillation (HD) and supercritical \(CO_{2}\) extraction (\(ESCO_{2}\)). The obtained isolates were analyzed by coupled gas chromatography and mass spectrometry (GC-MS). Furthermore, the fatty acid content was analyzed by gas chromatography with a flame ionization detector (GC-FID). The pigments were extracted and purified using solid phase extraction (SPE) and \(ESCO_{2}\) from freeze-dried macroalgal samples. In the obtained purified fractions and \(CO_{2}\) extracts, the pigments were identified and quantified by high performance liquid chromatography (HPLC). In addition, the concentrations of total chlorophylls and carotenoids in the obtained SPE fractions and \(CO_{2}\) extracts were determined by spectrophotometric method. Based on the obtained results, significant differences were observed between different types of macroalgae. During the determination of the profile of volatile compounds, it was found that the influence of air drying plays a significant role on the composition of the present compounds. Also, degradation products of fatty acids and pigments were observed, which indicate oxidation processes during drying. The macroalgae used in this study can be considered as sources of high-value ω-3 and ω-6 fatty acids that were present in all three macroalgae. The results showed that characteristic pigments for a particular group of macroalgae were present. Fucoxanthin was detected as the dominant pigment in brown alga F. virsoides, chlorophyll a and β-carotene were dominant in red alga A. rigida, while in green alga C. bursa chlorophyll b and astaxanthin were present. This research significantly contributes to a better understanding of the chemical biodiversity of macroalgae from the Adriatic Sea and their potential for application in the food, cosmetic and/or pharmaceutical industries.