Application of high‐speed counter‐current chromatography and HPLC to separate and purify of three polyacetylenes from Platycodon grandiflorum

Abstract

Three polyacetylenes were isolated and purified from Platycodon grandiflorum A. DC for the first time by high-speed counter-current chromatography using a two-phase solvent system composed of hexane/ethyl acetate/methanol/water (1:31:1:31, v/v/v/v) and high-performance liquid chromatography with an Agilent ZORBAX® SB-C18 column (4.6 mm × 150 mm, 5 μm). After separation by high-speed counter-current chromatography and high-performance liquid chromatography, we obtained 3.5 mg of platetyolin A, 4.1 mg of platetyolin B, and 18.1 mg of lobetyolin with purities of 97.2, 96.7, and 96.9%, respectively. The purity of each compound was assessed by high-performance liquid chromatography and the chemical structures were evaluated by high-resolution electrospray ionization time-of-flight mass spectrometry and one- and two-dimensional NMR spectroscopy. Among the isolated compounds, platetyolin A and platetyolin B are newly reported compounds.

Separation of five diketopiperazines from the marine fungus Alternaria alternate HK‐25 by high‐speed counter‐current chromatography

“…High-speed counter-current chromatography (HSCCC) is a liquid-liquid partition chromatography method that can receive pure compounds from crude samples with higher efficiency and recovery, which eliminates irreversible adsorption by solid support media [16][17][18]. In addition, in comparison with the conventional column separation methods, HSCCC is a preparative technique with a wide range of the solvent systems for scaling up [18], and this method has been widely F I G U R E 1 Structures of 12,13-dihydroxy-fumitremorgin C (1), gliotoxin (2), demethoxyfumitremorgin C (3), bisdethiobis(methylthio)gliotoxin (4), fumitremorgin C (5) used for isolation of natural products [19][20][21][22]. In published papers, three sulfur-containing DKPs and other DKPs were successfully separated by HSCCC [23,24].…”

A practicable strategy for enrichment and separation of four minor flavonoids including two isomers from barley seedlings by macroporous resin column chromatography, medium‐pressure LC, and high‐speed countercurrent chromatography

“…The advantages of this technique include convenience, high adsorption capacity, low operational expense, less solvent consumption, the absence of chemical residues in the product, and easy regeneration . More importantly, crude extracts could be applied directly . Thus, macroporous resin column chromatography (MRCC) is selected to treat the crude extract before MPLC enrichment process.…”

Combined chromatographic strategy based on macroporous resin, high‐speed counter‐current chromatography and preparative HPLC for systematic separation of seven antioxidants from the fruit of Terminalia billerica

“…The advantages of this technique includes convenience, high adsorption capacity, low operational expense, less solvent consumption, absence of chemical residues in the product, and easy regeneration . Besides, crude extracts could be applied directly . More importantly, target elution is feasible by modifying the elution conditions.…”