title: Rapid isolation, reliable characterization, and water solubility improvement of polymethoxyflavones from cold-pressed mandarin essential oil.
abstract: Polymethoxyflavones possess many biological properties, as lipid-lowering, hypoglycaemic, anti-inflammatory, antioxidant, and anticancer activities, therefore, they may be employed as nutraceuticals or therapeutic agents. The scarcity of pure polymethoxyflavones on the market as well as their low water solubility limited in vivo studies and the use of polymethoxyflavones as food or pharmaceutical supplements. Since mandarin peels are a rich source of polymethoxyflavones, tangeretin, nobiletin, sinensetin, tetra-O-methyl scutellarein, and heptamethoxyflavone were purified from a nonvolatile residue of a cold-pressed mandarin essential oil using a multidimensional preparative liquid chromatographic system coupled with a photodiode array detector and a single quadrupole mass spectrometer. A new prototype, consisting of a nano-liquid chromatography system coupled with an electron ionization mass spectrometer, was used for the characterization of the pure isolated molecules. Finally, due to the collection of highly pure nobiletin and tangeretin, the ability of 2-hydroxypropyl-β-cyclodextrin to enhance the water solubility of both polymethoxyflavones was evaluated by phase solubility studies and Job's plot method.
authors.affiliation: "Scienze chimiche, biologiche, farmaceutiche ed ambientali" Department, University of Messina, Messina, Italy.|Chromaleont s.r.l, c/o, University of Messina, Messina, Italy.|University Campus Bio-Medico of Rome, Rome, Italy.
authors.forename: Marina
authors.initials: M
authors.lastname: Russo
authors.affiliation: "Scienze chimiche, biologiche, farmaceutiche ed ambientali" Department, University of Messina, Messina, Italy.
authors.forename: Francesca
authors.initials: F
authors.lastname: Rigano
authors.affiliation: "Scienze chimiche, biologiche, farmaceutiche ed ambientali" Department, University of Messina, Messina, Italy.
authors.forename: Adriana
authors.initials: A
authors.lastname: Arigò
authors.affiliation: "Scienze chimiche, biologiche, farmaceutiche ed ambientali" Department, University of Messina, Messina, Italy.
authors.forename: Danilo
authors.initials: D
authors.lastname: Sciarrone
authors.affiliation: "Scienze chimiche, biologiche, farmaceutiche ed ambientali" Department, University of Messina, Messina, Italy.
authors.forename: Maria Luisa
authors.initials: ML
authors.lastname: Calabrò
authors.affiliation: Division of Cellular Transplantation of surgery, Diabetes Research Institute, University of Miami, Miami, FL, USA.
authors.forename: Sara
authors.initials: S
authors.lastname: Farnetti
authors.affiliation: "Scienze chimiche, biologiche, farmaceutiche ed ambientali" Department, University of Messina, Messina, Italy.|Chromaleont s.r.l, c/o, University of Messina, Messina, Italy.|University Campus Bio-Medico of Rome, Rome, Italy.
authors.forename: Paola
authors.initials: P
authors.lastname: Dugo
authors.affiliation: "Scienze chimiche, biologiche, farmaceutiche ed ambientali" Department, University of Messina, Messina, Italy.|Chromaleont s.r.l, c/o, University of Messina, Messina, Italy.|University Campus Bio-Medico of Rome, Rome, Italy.
authors.forename: Luigi
authors.initials: L
authors.lastname: Mondello
mesh_terms: D002851:Chromatography, High Pressure Liquid; D002957:Citrus / Q000737:chemistry*; D003080:Cold Temperature; D047309:Flavones / Q000737:chemistry* / Q000302:isolation & purification*; D005638:Fruit / Q000737:chemistry; D009822:Oils, Volatile / Q000737:chemistry*; D011108:Polymers / Q000737:chemistry*; D012984:Software; D012995:Solubility; D014867:Water / Q000737:chemistry*
chemical_list: D047309:Flavones; D009822:Oils, Volatile; D011108:Polymers; D014867:Water
keywords: Mandarin; Miniaturized liquid chromatography; Multidimensional chromatography; Polymethoxyflavones; Preparative high-performance liquid chromatography