Journal
MOLECULES
Volume 18, Issue 10, Pages 12896-12908Publisher
MDPI
DOI: 10.3390/molecules181012896
Keywords
preparative separation; spirobisnaphthalenes; endophytic fungus; Berkleasmium sp Dzf12; high-speed counter-current chromatogrphy
Funding
- National Natural Science Foundation of China [31071710]
- program for Changjiang Scholars and Innovative Research Team in University of China [IRT1042]
- Hi-Tech R&D Program of China [2011AA10A202]
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High-speed counter-current chromatography (HSCCC) was applied for the first time for the preparative separation of spirobisnaphthalenes from a crude extract of the endophytic fungus Berkleasmium sp. Dzf12, associated with the medicinal plant Dioscorea zingiberensis. Six spirobisnaphthalenes were successfully separated by HSCCC with a two-phase solvent system composed of n-hexane-chloroform-methanol-water (1.5:3.0:2.5:2.0, v/v). About 18.0 mg of diepoxin kappa (1), 245.7 mg of palmarumycin C-13 (2), 42.4 mg of palmarumycin C-16 (3), 42.2 mg of palmarumycin C-15 (4), 32.6 mg of diepoxin delta (5), and 22.3 mg of diepoxin gamma (6) with purities of 56.82, 71.39, 76.57, 75.86, 91.01 and 82.48%, respectively, as determined by high-performance liquid chromatography (HPLC), were obtained from 500 mg of the crude extract in a one-step elution within 7 h of separation procedure by HSCCC. The purified spirobisnaphthalenes were further structurally characterized by means of physicochemical and spectrometric analysis.
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