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.

Antimicrobial activity of puffball(Bovistella radicata) and separation of bioactive compounds

“…According to established protocols (Tian et al 2011; Zhang et al 2012; Sen et al 2014), each 10 mg mixed puffball powder were extracted by 200 ml ethanol/aqueous/chloroform/n-butanol/Aether/Ethyl acetate for continuously 10 h. After filtration over Whatman No. 4 paper, the extracts were concentrated under a reduced pressure at 40 °C and stored at 4 °C in sterile bottles for further use.…”

Adsorption/desorption characteristics, separation and purification of phenazine‐1‐carboxylic acid from fermentation extract by macroporous adsorbing resins

“…The adsorption characteristics of macroporous resins, especially for the separation of aromatic compounds, include polarity, surface area, and pore diameter. These properties are primarily based on electrostatic interaction, hydrogen bonding, complexation, and size sieving action between polymeric adsorbents and solutes from the solution …”

“…These properties are primarily based on electrostatic interaction, hydrogen bonding, complexation, and size sieving action between polymeric adsorbents and solutes from the solution. 25,31 Previously, macroporous resins have been successfully applied to separate and purify a broad spectrum of macromolecules and chemical entities including alkaloids, coumarins, chlorogenic acid, 32 polyphenolics (resveratrol) and terpenoids, 33 flavonoids, 34,35 flavone glucuronides, 25 lycopene, 36,37 lignans and saponins, 38 and spiropreussione A 39 from aqueous solutions and fermentation broths. However, to the best of our knowledge, no report has been documented yet on the isolation and purification of PCA by macrospores resins.…”

Elution–extrusion counter‐current chromatography for the separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix

“…In recent years, highspeed counter-current chromatography (HSCCC), which can eliminate irreversible absorptive loss of samples and offers high resolution comparable to column chromatography, has been widely used in fast separation and purification of chemical components from Chinese medicinal herbs [23][24][25][26]. Further, elution-extrusion counter-current chromatography (EECCC), which combines normal elution and extrusion in a single run, was developed by Berthod [27].…”