期刊
JOURNAL OF SEPARATION SCIENCE
卷 43, 期 13, 页码 2646-2656出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201901245
关键词
cadinene sesquiterpenoids; Eupatorium adenophorum Spreng; industrial preparative chromatography; molecular distillation; supercritical fluid extraction
资金
- National Key R&D Program of China [2017YFC1703102]
A green and efficient strategy was established and optimized for target-oriented extraction, enrichment and separation of cadinene sesquiterpenoids from Eupatorium adenophorum Spreng., using the combination of supercritical fluid extraction, molecular distillation, and industrial preparative chromatography for the first time. The extraction conditions of supercritical fluid extraction were initially optimized by orthogonal experimental design. Under the optimum conditions, the contents of 9-oxo-10,11-dehydroageraphorone and 10H beta-9-oxo-ageraphorone, which were 55.00% and 6.01%, respectively, were much higher than conventional extraction methods. Then, the molecular distillation enrichment method was established and investigated by response surface methodology technology, which showed strong specificity for enriching target compounds and removing impurities from crude extracts. Under the optimum conditions of molecular distillation, total contents of cadinene sesquiterpenoids were increased to 89.19%. Finally, a total of 146 mg of 9-oxo-10,11-dehydroageraphorone and 29 mg of 10H beta-9-oxo-ageraphorone were easily obtained by industrial preparative chromatography, from 200 mg of distillation fraction, with purities over 99%. The contents of target components were analyzed by HPLC, and structures of them were identified by high-resolution MS, H-1-NMR, and C-13-NMR spectroscopy. These results indicate that it is a simple, effective, and eco-friendly strategy, which is easily converted into industrial scale.
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