Separation and purification of neohesperidin from the albedo of Citrus reticulata cv. Suavissima by combination of macroporous resin and high‐speed counter‐current chromatography
Identifieur interne : 001462 ( Main/Exploration ); précédent : 001461; suivant : 001463Separation and purification of neohesperidin from the albedo of Citrus reticulata cv. Suavissima by combination of macroporous resin and high‐speed counter‐current chromatography
Auteurs : Jiukai Zhang [République populaire de Chine] ; Xiaoyan Zhu [République populaire de Chine] ; Fenglei Luo [République populaire de Chine] ; Chongde Sun [République populaire de Chine] ; Jianzhen Huang [République populaire de Chine] ; Xian Li [République populaire de Chine] ; Kunsong Chen [République populaire de Chine]Source :
- Journal of Separation Science [ 1615-9306 ] ; 2012-01.
English descriptors
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.
Url:
DOI: 10.1002/jssc.201100695
Affiliations:
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Le document en format XML
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<front><div type="abstract" xml:lang="en">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.</div>
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