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Open AccessArticle

Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction

by Fengwei He 1, Li Chen 1, Qian Liu 2, Xiao Wang 2, Jia Li 3,* and Jinqian Yu 2,*
1
Liaoning Institute of Science and Technology, Benxi 117004, China
2
Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, China
3
College of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250355, China
*
Authors to whom correspondence should be addressed.
Molecules 2018, 23(12), 3353; https://doi.org/10.3390/molecules23123353
Received: 21 November 2018 / Revised: 12 December 2018 / Accepted: 16 December 2018 / Published: 18 December 2018
Three phenylethanoid glycosides, echinacoside (1), salidroside (3), and acteoside (6), and three secoiridoid glycosides, isonuezhenide (2), nuezhenoside G13 (4), and specnuezhenide (5), 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 4 and 5 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 1, 4.5 mg of compound 2, 6.8 mg of compound 3, 5.9 mg of compound 4, 11.2 mg of compound 5, and 2.2 mg of compound 6 in one separation run under the solvent system of ethyl acetate:n-butanol:water (2:1:3, v/v) from 200 mg of the UPE extract. The structures of these phenylethanoid and secoiridoid glycosides were elucidated by extensive spectroscopic methods. View Full-Text
Keywords: high-speed counter-current chromatography; phenylethanoid glycoside; secoiridoid glycoside Ligustri Lucidi Fructus; ultrahigh pressure extraction high-speed counter-current chromatography; phenylethanoid glycoside; secoiridoid glycoside Ligustri Lucidi Fructus; ultrahigh pressure extraction
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He, F.; Chen, L.; Liu, Q.; Wang, X.; Li, J.; Yu, J. Preparative Separation of Phenylethanoid and Secoiridoid Glycosides from Ligustri Lucidi Fructus by High-Speed Counter-Current Chromatography Coupled with Ultrahigh Pressure Extraction. Molecules 2018, 23, 3353.

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