Some experiments were conducted to optimize the extraction conditions in the reference describing SPME hop cones analysis (Kovačevič and Kač 2001). In the current work for SPME method 0.2 g of dry hop cones were taken. Dry hop cones were mixed with 2 ml of distilled water into vial. SPME device (Supelco Inc., Bellefonte, PA, USA) with polydimethylsiloxane (PDMS) fiber of 100 μm thickness was used for the determination of analytes. The headspace vials (5 ml volume) were used for extractions. Sample preparation conditions were as follows: extraction time 45 min, and extraction temperature 60 °C. The temperature of SPME extraction was obtained by thermocirrculator Julabo