期刊
JOURNAL OF SEPARATION SCIENCE
卷 42, 期 15, 页码 2510-2516出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201801284
关键词
Alternaria alternate; diketoperazines; high-speed counter-current chromatography; solvent selection
资金
- National Key Research and Development Program of China [2018YFC0310900]
- National Natural Science Foundation of China [41776168, 41706167]
- Ningbo Public Service Platform for High-Value Utilization of Marine Biological Resources [NBHY-2017-P2]
- Zhejiang Provincial Public Welfare Technology Program [LGC19B020002]
- Natural Science Foundation of Ningbo [2018A610303, 2018A610320]
- National 111 Project of China [D16013]
- Li Dak Sum Yip Yio Chin Kenneth Li Marine Biopharmaceutical Development Fund
- K.C. Wong Magna Fund in Ningbo University
High-speed counter-current chromatography was applied to the separation of five diketoperazines from the marine Alternaria alternate HK-25 for the first time using one-step elution method with a pair of two-phase solvent systems composed of petroleum ether/ethyl acetate/methanol/water (5.5:11:5:7, v/v). Where 151.6 mg of crude sample yielded five diketoperazines, 12,13-dihydroxy-fumitremorgin C (1), gliotoxin (2), demethoxyfum itremorgin C (3), bisdethiobis(methylthio)gliotoxin (4), fumitremorgin C (5), and the purities of all compounds were above 94% as determined by high-performance liquid chromatography. The structures of these compounds were identified by H-1 and C-13 NMR spectroscopy. These results showed that high-speed counter-current chromatography can provide a feasible way for highly effective preparation of marine natural products, which ensured the supple of numerous samples for drug development.
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