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Molecules 2016, 21(8), 1016; doi:10.3390/molecules21081016

Preparative Separation of Phenolic Compounds from Chimonanthus praecox Flowers by High-Speed Counter-Current Chromatography Using a Stepwise Elution Mode

1
College of Pharmacy, Shandong University of Traditional Chinese Medicine, 4655 Daxue Street, Jinan 250355, Shandong, China
2
Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, Shandong, China
3
Kangsen Sanfeng Biological Engineering Technology Co., Jinan 250014, Shandong, China
*
Authors to whom correspondence should be addressed.
Academic Editor: Derek J. McPhee
Received: 29 June 2016 / Revised: 25 July 2016 / Accepted: 31 July 2016 / Published: 4 August 2016
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Abstract

High-speed counter-current chromatography (HSCCC) has been successfully used for the separation of eight compounds from Chimonanthus praecox flowers. Firstly, the crude extract of Chimonanthus praecox flowers was dissolved in a two-phase solvent system composed of petroleum ether–ethyl acetate–methanol–H2O (5:5:3:7, v/v) and divided into two parts: the upper phase (part I) and the lower phase (part II). Then, HSCCC was applied to separate the phenolic acids from part I and part II, respectively. Considering the broad polarity range of target compounds in part I, a stepwise elution mode was established. Two optimal solvent systems of petroleum ether–ethyl acetate–methanol–H2O–formic acid (FA) (5:5:3:7:0.02, 5:5:4.3:5.7:0.02, v/v) were employed in this separation. Five phenylpropanoids and two flavonoids were successfully separated from 280 mg of part I, including 8.7 mg of 3,4-dihydroxy benzoic acid (a, 95.3% purity), 10.9 mg of protocatechualdehyde (b, 96.8% purity), 11.3 mg of p-coumaric acid (c, 98.9% purity), 12.2 mg of p-hydroxybenzaldehyde (d, 95.9% purity), 24.7 mg of quercetin (e, 97.3% purity), 33.8 mg of kaempferol (f, 96.8% purity), and 24.6 mg of 4-hydroxylcinnamic aldehyde (g, 98.0% purity). From 300 mg of part II, 65.7 mg of rutin (h, 98.2% purity), 7.5 mg of 3,4-dihydroxy benzoic acid (a, 77.4% purity), and 4.7 mg of protocatechualdehyde (b, 81.6% purity) were obtained using the solvent system EtOAc–n-butanol (n-BuOH)–FA–H2O (4:1:0.5:5, v/v). The structures of the eight pure compounds were confirmed by electrospray ionization-mass spectrometry (ESI-MS), 1H-NMR and 13C-NMR. To the best of our knowledge, compounds ad and f were the first separated and reported from the Chimonanthus praecox flower extract. View Full-Text
Keywords: preparative separation; phenolic compounds; Chimonanthus praecox flower; high-speed counter-current chromatography (HSCCC); stepwise elution mode preparative separation; phenolic compounds; Chimonanthus praecox flower; high-speed counter-current chromatography (HSCCC); stepwise elution mode
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Li, H.; Zhang, Y.; Liu, Q.; Sun, C.; Li, J.; Yang, P.; Wang, X. Preparative Separation of Phenolic Compounds from Chimonanthus praecox Flowers by High-Speed Counter-Current Chromatography Using a Stepwise Elution Mode. Molecules 2016, 21, 1016.

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