Purification of Spent Hop Cone (Humulus lupulus L.) Extract with Xanthohumol Using Mesoporous Superparamagnetic Iron...

(1) Background: Over 90% of hop crops are currently used in beer production, with a small part used in the cosmetics and pharmaceutical industries. Spent hops as a waste product contain one of the strongest antioxidants, xanthohumol. The aim of the study was to purify spent hop extracts by magnetic dispersive extraction using iron oxide nanoparticles (IONP) to obtain pure xanthohumol; (2) Methods: The extract from the waste product obtained after supercritical carbon dioxide extraction of hops was prepared by ultrasound-assisted extraction utilizing different solvents, i.e., ethyl acetate, propanol, acetone, 80% methanol, ethyl acetate-methanol (1:1, v/v), and propanol-methanol (1:1, v/v). The hydrodynamic diameters and zeta potential of IONPs before and after incubation were measured by dynamic light scattering (DLS). The extracts were analyzed by reversed-phase high-performance liquid chromatography (HPLC). Isolated xanthohumol was identified based on the DAD spectrum in the range of 200-600 nm and by Fourier transform infrared spectroscopy/attenuated total reflectance (FT-IR/ATR); The antioxidant activity of extracts before and after incubation with IONPs was assessed using SNPAC (Silver Nanoparticle Antioxidant Capacity), DPPH (2,2-diphenyl-1-picrylhydrazyl radical), and FRAP (Ferric Reducing Antioxidant Power) assays, as well as total phenolic content (TPC) and total flavonoid content (TFC). (3) Results: The amount of added IONPs, the kind of solvent, and the contact time of the extract with nanoparticles were optimized. We found that 80% MeOH extract after incubation with IONPs (865 µg IONPs/g of spent hops) at room temperature for 48 h contains 74.61% of initial xanthohumol content, providing a final xanthohumol concentration of 43 µg mL^-1. (4) Conclusions: The proposed method of magnetic dispersive extraction using IONPs allows for the purification of spent hops extract and obtaining a pure product, namely xanthohumol, with a wide potential for practical applications in medicine, pharmacy, cosmetics, and agriculture. This is clear evidence of the usefulness of IONP as an effective sorbent. The method allows the use of residues from the brewing industry, i.e., the biomass of used hop cones to obtain a valuable substance.