Fractionation of High-Value Compounds from Hops Using an Optimised Sequential Extraction Procedure

This study describes the development and optimisation of a process for the extraction and fractionation of high-value compounds from hops. Firstly, the efficacy of ten organic solvents was compared for performing the initial solid–liquid extraction of compounds from hop pellets with subsequent fractionation steps. A methanol–dichloromethane mixture was selected and the extraction variables were optimised in order to maximise the recovery of valuable hop compounds separated into different streams (α- and β-acids in soft resins, xanthohumol in hard resins, and phenolics in spent solids) after fractionation steps. The optimisation results showed that extraction of hop pellets performed at room temperature with 19.7% (v/v) methanol for 89 min yielded recoveries of 86.57% α-acids and 89.14% β-acids in soft resins, 78.48% xanthohumol in hard resins and 67.10% phenolics in spent solids. These conditions were successfully validated using six hop varieties. Moreover, the antioxidant properties of all recovered fractions were compared and the soft resins showed the highest antioxidant activities, reaching values of 3.91 ± 0.10 g AAE/100 g for ferric reducing power (FRAP) and 0.10 ± 0.01 mg/mL for 50% of radical scavenging activity (EC50). The optimised sequential extraction could serve as a basis for larger scale-up for industrial production.