title: Separation and purification of neohesperidin from the albedo of Citrus reticulata cv. Suavissima by combination of macroporous resin and high-speed counter-current chromatography.
abstract: In this article, a simple and efficient protocol for rapid preparation and separation of neohesperidin from the albedo of Citrus reticulata cv. Suavissima was established by the combination of macroporous resin column chromatography and high-speed counter-current chromatography (HSCCC). Six types of resin were investigated by adsorption and desorption tests, and D101 macroporous resin was selected for the first cleaning-up procedure, in which 55% aqueous ethanol was used to elute neohesperidin. After treatment with D101 resin, the neohesperidin purity increased 11.83-fold from 4.92% in the crude extract to 58.22% in the resin-refined sample, with a recovery of 68.97%. The resin-refined sample was directly subjected to HSCCC purification with a two-phase solvent system composed of ethyl acetate-n-butanol-water (4:1:5, v/v), and 23.6 mg neohesperidin with 97.47% purity was obtained from 60 mg sample in only one run. The recovery of neohesperidin in HSCCC separation procedure was 65.85%. The chemical structure of the purified neohesperidin was identified by both HPLC and LC-MS. The established purification process will be helpful for further characterization and utilization of Citrus neohesperidin.
authors.affiliation: Laboratory of Fruit Quality Biology/The State Agriculture Ministry Laboratory of Horticultural Plant Growth, Development and Quality Improvement, Zhejiang University, Hangzhou, Zhejiang Province, P. R. China.
authors.forename: Jiukai
authors.initials: J
authors.lastname: Zhang
authors.forename: Xiaoyan
authors.initials: X
authors.lastname: Zhu
authors.forename: Fenglei
authors.initials: F
authors.lastname: Luo
authors.forename: Chongde
authors.initials: C
authors.lastname: Sun
authors.forename: Jianzhen
authors.initials: J
authors.lastname: Huang
authors.forename: Xian
authors.initials: X
authors.lastname: Li
authors.forename: Kunsong
authors.initials: K
authors.lastname: Chen
mesh_terms: D002845:Chromatography / Q000295:instrumentation / Q000379:methods*; D002957:Citrus / Q000737:chemistry*; D003377:Countercurrent Distribution / Q000295:instrumentation / Q000379:methods*; D006569:Hesperidin / Q000031:analogs & derivatives* / Q000737:chemistry / Q000302:isolation & purification; D015394:Molecular Structure; D010936:Plant Extracts / Q000737:chemistry / Q000302:isolation & purification*; D012117:Resins, Synthetic / Q000737:chemistry
chemical_list: D010936:Plant Extracts; D012117:Resins, Synthetic; D006569:Hesperidin; C546526:neohesperidin