The distillation of essential oil produces hydrolate or aromatic water as a by-product, which contains volatile compounds that contribute to its aromatic and therapeutic properties. The aim of this study was to isolate and identify the volatile compounds from the hydrolates of lavender (Lavandula angustifolia), immortelle (Helichrysum italicum) and geranium (Pelargonium graveolens). Two extraction techniques were used for this purpose: Headspace solid- phase microextraction (HS-SPME) and extraction by mixing with a magnetic stirrer. The headspaces and extracts were analysed using a coupled gas chromatography-mass spectrometry (GC-MS) system. The results showed that the different extraction techniques led to different profiles of the volatile compounds. Headspace extraction enabled the isolation of key compounds such as linalool and citronellol, while extraction by mixing yielded a wider range of compounds, including heavier and less volatile ones. The proportion of total identified compounds obtained by headspace solid-phase extraction was higher in all hydrolates. The results of this study confirm that the most abundant compounds include terpenes, which are responsible for characteristic odours and often have antimicrobial and anti-inflammatory properties, and phenols, which contribute to the aromatic profile and may have strong antioxidant properties. The results show that the choice of extraction techniques to isolate volatile compounds significantly influences their quality and quantity, which is crucial for applications in aromatherapy and the fragrance industry. The quality of volatile compounds can contribute to specific fragrance profiles and therapeutic properties, while a greater quantity of isolated compounds can increase product efficacy.