An efficient combination of supercritical fluid extraction and high-speed counter-current chromatography to extract and purify homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler | |
Ma, Chengjun1; Li, Gang1; Zhang, Juan1; Zheng, Qiusheng1; Fan, Xiao2; Wang, Zhenhua3 | |
2009-06-01 | |
发表期刊 | JOURNAL OF SEPARATION SCIENCE |
ISSN | 1615-9306 |
卷号 | 32期号:11页码:1949-1956 |
文章类型 | Article |
摘要 | Supercritical fluid extraction (SFE) was used to extract homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler. The optimization of parameters was carried out using an orthogonal test L(9) (3)(4) including pressure, temperature, dynamic extraction time and the amount of modifier. The process was then scaled up by 100 times with a preparative SFE system under the optimized conditions of 25 MPa, 55 degrees C, 4.0 h and 25% methanol as a modifier. Then crude extracts were separated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/ACN/water (1.8:1.0:1.0:1.2:1.0 v/v). There three homoisoflavonoidal compounds including methylophiopogonanone A 6-aldehydo-isoophiopogonone A, and 6-formyl-isoophiopogonanone A, were successfully isolated and purified in one step. The collected fractions were analyzed by HPLC. In each operation, 140 mg crude extracts was separated and yielded 15.3 mg of methylophiopogonanone A (96.9% purity), 4.1 mg of 6-aldehydo-isoophiopogonone A (98.3% purity) and 13.5 mg of 6-formyl-isoophiopogonanone A (97.3% purity) respectively. The chemical structure of the three homoisoflavonoids are identified by means of ESI-MS and NMR analysis.; Supercritical fluid extraction (SFE) was used to extract homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler. The optimization of parameters was carried out using an orthogonal test L-9 (3)(4) including pressure, temperature, dynamic extraction time and the amount of modifier. The process was then scaled up by 100 times with a preparative SFE system under the optimized conditions of 25 MPa, 55 degrees C, 4.0 h and 25% methanol as a modifier. Then crude extracts were separated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/ACN/water (1.8:1.0:1.0:1.2:1.0 v/v). There three homoisoflavonoidal compounds including methylophiopogonanone A 6-aldehydo-isoophiopogonone A, and 6-formyl-isoophiopogonanone A, were successfully isolated and purified in one step. The collected fractions were analyzed by HPLC. In each operation, 140 mg crude extracts was separated and yielded 15.3 mg of methylophiopogonanone A (96.9% purity), 4.1 mg of 6-aldehydo-isoophiopogonone A (98.3% purity) and 13.5 mg of 6-formyl-isoophiopogonanone A (97.3% purity) respectively. The chemical structure of the three homoisoflavonoids are identified by means of ESI-MS and NMR analysis. |
关键词 | High-speed Counter-current Chromatography Homoisoflavonoids Ophiopogon Japonicus Plant Material Supercritical Fluid Extraction |
学科领域 | Chemistry, Analytical |
DOI | 10.1002/jssc.200800732 |
URL | 查看原文 |
收录类别 | SCI |
语种 | 英语 |
WOS记录号 | WOS:000266929700020 |
引用统计 | |
文献类型 | 期刊论文 |
条目标识符 | http://ir.qdio.ac.cn/handle/337002/3478 |
专题 | 海洋生物技术研发中心 |
作者单位 | 1.Yantai Univ, Dept Bioengn, Coll Ocean, Yantai 264003, Shandong, Peoples R China 2.Chinese Acad Sci, Inst Oceanol, Qingdao, Peoples R China 3.Shihezi Univ, Coll Pharm, Shihezi, Peoples R China |
推荐引用方式 GB/T 7714 | Ma, Chengjun,Li, Gang,Zhang, Juan,et al. An efficient combination of supercritical fluid extraction and high-speed counter-current chromatography to extract and purify homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler[J]. JOURNAL OF SEPARATION SCIENCE,2009,32(11):1949-1956. |
APA | Ma, Chengjun,Li, Gang,Zhang, Juan,Zheng, Qiusheng,Fan, Xiao,&Wang, Zhenhua.(2009).An efficient combination of supercritical fluid extraction and high-speed counter-current chromatography to extract and purify homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler.JOURNAL OF SEPARATION SCIENCE,32(11),1949-1956. |
MLA | Ma, Chengjun,et al."An efficient combination of supercritical fluid extraction and high-speed counter-current chromatography to extract and purify homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler".JOURNAL OF SEPARATION SCIENCE 32.11(2009):1949-1956. |
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