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Separation of five diketopiperazines from the marine fungus Alternaria alternate HK‐25 by high‐speed counter‐current chromatography
Author(s) -
He Xiaoping,
Ding Lijian,
Yi Mengqi,
Xu Jianzhou,
Zhou Xuezhen,
Zhang Weiyan,
He Shan
Publication year - 2019
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201801284
Subject(s) - countercurrent chromatography , chromatography , diketopiperazines , chemistry , gliotoxin , alternaria , petroleum ether , elution , high performance liquid chromatography , methanol , ethyl acetate , extraction (chemistry) , organic chemistry , botany , aspergillus fumigatus , biology
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 1 H and 13 C 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.