title: Metabolite profiling of polyphenols in peels of Citrus limetta Risso by combination of preparative high-speed countercurrent chromatography and LC-ESI-MS/MS.
abstract: The polar constituents of peels from Citrus limetta variety Risso (Rutaceae) were investigated by a combination of two complementary chromatographic techniques consisting of preparative high-speed countercurrent chromatography (HSCCC), and off-line LC-ESI-MS/MS analysis to design a two-dimensional metabolite profile. Countercurrent chromatography (CCC) using solely immiscible solvent systems allowed the fractionation of principal components and an enrichment of minor concentrated metabolites from a crude polar solvent partition of C. limetta peels for subsequent structural identification by LC-ESI-MS/MS analysis. The combination of two very different chromatographic techniques resulted in lower detection limits for electrospray mass-spectrometry and revealed eighty-five compounds, including three abscisic acid derivatives, five limonoid glycosides, twenty-six dihydro-cinnamic and cinnamic acid glycosides, eleven flavanone glycosides, seven flavone glycosides, seventeen flavonol glycosides, including limocitrol and limocitrin derivatives. As a chemocharacteristic for C. limetta metabolites, many of the detected structures were linked to single and multiple 3-hydroxy-3-methyl-glutaryl (HMG) substitutions. C. limetta peels are a by-product of juice production, and not only the antioxidant fractions but also some of the fortified compounds could be used for food and pharmaceutical purposes.
authors.affiliation: Departamento de Tecnología Alimentaria, Centro de Investigación y Asistencia en Tecnología y Diseño del Estado de Jalisco, Av. Normalistas 800, Colinas de la Normal, 44270 Guadalajara Jalisco, Mexico.
authors.forename: M Paulina
authors.initials: MP
authors.lastname: Rodríguez-Rivera
authors.affiliation: Departamento de Tecnología Alimentaria, Centro de Investigación y Asistencia en Tecnología y Diseño del Estado de Jalisco, Av. Normalistas 800, Colinas de la Normal, 44270 Guadalajara Jalisco, Mexico.
authors.forename: Eugenia
authors.initials: E
authors.lastname: Lugo-Cervantes
authors.affiliation: Institute of Food Chemistry, Technische Universität Braunschweig, Schleinitzstrasse 20, 38106 Braunschweig, Germany.
authors.forename: Peter
authors.initials: P
authors.lastname: Winterhalter
authors.affiliation: Institute of Food Chemistry, Technische Universität Braunschweig, Schleinitzstrasse 20, 38106 Braunschweig, Germany. Electronic address: g.jerz@tu-bs.de.
authors.forename: Gerold
authors.initials: G
authors.lastname: Jerz
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D002957:Citrus / Q000737:chemistry*; D003377:Countercurrent Distribution / Q000379:methods*; D044948:Flavonols / Q000032:analysis; D006027:Glycosides / Q000737:chemistry; D013058:Mass Spectrometry / Q000379:methods*; D059808:Polyphenols
chemical_list: D044948:Flavonols; D006027:Glycosides; D059808:Polyphenols
keywords: Citrus limetta Risso; HMG-substituted polyphenols; LC–ESI–MS/MS; Preparative HSCCC; Rutaceae; Two-dimensional metabolite profiling