title: Preparative separation of spirobisnaphthalenes from endophytic fungus Berkleasmium sp. Dzf12 by high-speed counter-current chromatography.
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 κ (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.
authors.affiliation: MOA Key Laboratory of Plant Pathology, Department of Plant Pathology, College of Agronomy and Biotechnology, China Agricultural University, Beijing 100193, China. lgzhou@cau.edu.cn.
authors.forename: Tijiang
authors.initials: T
authors.lastname: Shan
authors.forename: Shiqiong
authors.initials: S
authors.lastname: Lu
authors.forename: Chao
authors.initials: C
authors.lastname: Luo
authors.forename: Ruiya
authors.initials: R
authors.lastname: Luo
authors.forename: Yan
authors.initials: Y
authors.lastname: Mou
authors.forename: Mingan
authors.initials: M
authors.lastname: Wang
authors.forename: Youliang
authors.initials: Y
authors.lastname: Peng
authors.forename: Ligang
authors.initials: L
authors.lastname: Zhou
mesh_terms: D001203:Ascomycota / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D059625:Liquid-Liquid Extraction / Q000379:methods; D000432:Methanol; D009281:Naphthalenes / Q000737:chemistry / Q000302:isolation & purification*; D012997:Solvents; D013056:Spectrophotometry, Ultraviolet; D013141:Spiro Compounds / Q000737:chemistry / Q000302:isolation & purification*; D014867:Water
chemical_list: D009281:Naphthalenes; D012997:Solvents; D013141:Spiro Compounds; D014867:Water; D000432:Methanol