The Meyer lilac, Syringa meyeri Palibin, Oleaceae, is an ornamental plant with flowers of an intense and intoxicating fragrance. Since the scent is a result of volatile compounds, the main goal of this study was to isolate and identify the volatile compounds of lilac flowers. The extraction technique selected was headspace solid-phase microextraction (HS-SPME), which is particularly suitable for samples with strong aromas like flowers. Headspace solid-phase microextraction (HS-SPME) from fresh and frozen plant material was performed using blue (CAR/PDMS) and gray fibers (DVB/CAR/PDMS) at temperatures of 50 °C and 60 °C. The headspace analysis was performed using coupled system gas chromatography-mass spectrometry (GC- MS). The qualitative and quantitative composition of the lilac flower headspace was similar regardless of the plant material (fresh or frozen), the fiber used (blue or gray), and the extraction temperature (50 °C or 60 °C), meaning that the main components were largely the same compounds. The primary volatile compound of the lilac flower was the sesquiterpene hydrocarbon (E,E)-α-farnesene. The results obtained in this study confirm that the profile of volatile compounds isolated using headspace solid-phase microextraction is primarily dependent on the type of fiber used and extraction parameters such as temperature. The gray fiber was more efficient for isolating volatile compounds from lilac flowers, regardless of the temperature at which the extraction was performed and whether fresh or frozen plant material was used for isolation. Furthermore, a higher temperature resulted in the isolation and identification of more compounds, regardless of the fiber used. Therefore, Headspace Solid - Phase Microextraction using the gray fiber and at a temperature of 60 °C extracted a more complete profile of the lilac flower's volatile compounds.