Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction
Three phenylethanoid glycosides, echinacoside (<b>1</b>), salidroside (<b>3</b>), and acteoside (<b>6</b>), and three secoiridoid glycosides, isonuezhenide (<b>2</b>), nuezhenoside G13 (<b>4</b>), and specnuezhenide (<b>5</b>),...
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MDPI AG
2018-12-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/23/12/3353 |
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| author | Fengwei He Li Chen Qian Liu Xiao Wang Jia Li Jinqian Yu |
| author_facet | Fengwei He Li Chen Qian Liu Xiao Wang Jia Li Jinqian Yu |
| author_sort | Fengwei He |
| collection | DOAJ |
| description | Three phenylethanoid glycosides, echinacoside (<b>1</b>), salidroside (<b>3</b>), and acteoside (<b>6</b>), and three secoiridoid glycosides, isonuezhenide (<b>2</b>), nuezhenoside G13 (<b>4</b>), and specnuezhenide (<b>5</b>), have been extracted and separated by a combined method of ultrahigh pressure extraction (UPE) and high-speed counter-current chromatography (HSCCC) from Ligustri Lucidi Fructus. For the UPE, the optimal extraction was developed with conditions including solvent of 90% ethanol, sample to solvent ratio of 1:20 g/mL, pressure of 200 MPa, and time of 2 min, which rendered the yields of compounds <b>4</b> and <b>5</b> were 15.0 and 78.0 mg/g, respectively. For the HSCCC separation, the strategy of changing flow rates between 1.0 and 2.0 mL/min allowed the acquisition for 2.7 mg of compound <b>1</b>, 4.5 mg of compound <b>2</b>, 6.8 mg of compound <b>3</b>, 5.9 mg of compound <b>4</b>, 11.2 mg of compound <b>5</b>, and 2.2 mg of compound <b>6</b> in one separation run under the solvent system of ethyl acetate:<i>n</i>-butanol:water (2:1:3, <i>v</i>/<i>v</i>) from 200 mg of the UPE extract. The structures of these phenylethanoid and secoiridoid glycosides were elucidated by extensive spectroscopic methods. |
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| language | English |
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| spelling | doaj.art-e13ef7ae8e2e44e38fb1cdfea5225a092022-12-22T03:35:59ZengMDPI AGMolecules1420-30492018-12-012312335310.3390/molecules23123353molecules23123353Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure ExtractionFengwei He0Li Chen1Qian Liu2Xiao Wang3Jia Li4Jinqian Yu5Liaoning Institute of Science and Technology, Benxi 117004, ChinaLiaoning Institute of Science and Technology, Benxi 117004, ChinaShandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, ChinaShandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, ChinaCollege of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250355, ChinaShandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, ChinaThree phenylethanoid glycosides, echinacoside (<b>1</b>), salidroside (<b>3</b>), and acteoside (<b>6</b>), and three secoiridoid glycosides, isonuezhenide (<b>2</b>), nuezhenoside G13 (<b>4</b>), and specnuezhenide (<b>5</b>), have been extracted and separated by a combined method of ultrahigh pressure extraction (UPE) and high-speed counter-current chromatography (HSCCC) from Ligustri Lucidi Fructus. For the UPE, the optimal extraction was developed with conditions including solvent of 90% ethanol, sample to solvent ratio of 1:20 g/mL, pressure of 200 MPa, and time of 2 min, which rendered the yields of compounds <b>4</b> and <b>5</b> were 15.0 and 78.0 mg/g, respectively. For the HSCCC separation, the strategy of changing flow rates between 1.0 and 2.0 mL/min allowed the acquisition for 2.7 mg of compound <b>1</b>, 4.5 mg of compound <b>2</b>, 6.8 mg of compound <b>3</b>, 5.9 mg of compound <b>4</b>, 11.2 mg of compound <b>5</b>, and 2.2 mg of compound <b>6</b> in one separation run under the solvent system of ethyl acetate:<i>n</i>-butanol:water (2:1:3, <i>v</i>/<i>v</i>) from 200 mg of the UPE extract. The structures of these phenylethanoid and secoiridoid glycosides were elucidated by extensive spectroscopic methods.https://www.mdpi.com/1420-3049/23/12/3353high-speed counter-current chromatographyphenylethanoid glycosidesecoiridoid glycoside Ligustri Lucidi Fructusultrahigh pressure extraction |
| spellingShingle | Fengwei He Li Chen Qian Liu Xiao Wang Jia Li Jinqian Yu Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction Molecules high-speed counter-current chromatography phenylethanoid glycoside secoiridoid glycoside Ligustri Lucidi Fructus ultrahigh pressure extraction |
| title | Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction |
| title_full | Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction |
| title_fullStr | Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction |
| title_full_unstemmed | Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction |
| title_short | Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction |
| title_sort | preparative separation of phenylethanoid and secoiridoid glycosides from ligustri lucidi fructus by high speed counter current chromatography coupled with ultrahigh pressure extraction |
| topic | high-speed counter-current chromatography phenylethanoid glycoside secoiridoid glycoside Ligustri Lucidi Fructus ultrahigh pressure extraction |
| url | https://www.mdpi.com/1420-3049/23/12/3353 |
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