Abstract: 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 k (1), 245.7 mg of palmarumycin C13 (2), 42.4 mg of palmarumycin C16 (3), 42.2 mg of palmarumycin C15 (4), 32.6 mg of diepoxin δ (5), and 22.3 mg of diepoxin γ (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.
Keywords: preparative separation; spirobisnaphthalenes; endophytic fungus; Berkleasmium sp. Dzf12; high-speed counter-current chromatogrphy
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Shan, T.; Lu, S.; Luo, C.; Luo, R.; Mou, Y.; Wang, M.; Peng, Y.; Zhou, L. Preparative Separation of Spirobisnaphthalenes from Endophytic Fungus Berkleasmium sp. Dzf12 by High-Speed Counter-Current Chromatography. Molecules 2013, 18, 12896-12908.
Shan T, Lu S, Luo C, Luo R, Mou Y, Wang M, Peng Y, Zhou L. Preparative Separation of Spirobisnaphthalenes from Endophytic Fungus Berkleasmium sp. Dzf12 by High-Speed Counter-Current Chromatography. Molecules. 2013; 18(10):12896-12908.
Shan, Tijiang; Lu, Shiqiong; Luo, Chao; Luo, Ruiya; Mou, Yan; Wang, Mingan; Peng, Youliang; Zhou, Ligang. 2013. "Preparative Separation of Spirobisnaphthalenes from Endophytic Fungus Berkleasmium sp. Dzf12 by High-Speed Counter-Current Chromatography." Molecules 18, no. 10: 12896-12908.