Journal
PHYTOCHEMICAL ANALYSIS
Volume 22, Issue 4, Pages 352-360Publisher
WILEY-BLACKWELL
DOI: 10.1002/pca.1286
Keywords
HPLC-SPE-NMR; lignans; Phyllanthus myrtifolius; stilbenoids; Syagrus romanzoffiana; sample pretreatment; structural identification
Funding
- Ministry of Economics
- National Science Council, Taiwan, Republic of China [93-EC-17-A-20-S1-0010, NSC93-2320-B-002-024, NSC95-2320-B-002-034]
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Introduction - Application of on-line solid-phase extraction (SPE) as an interface between HPLC and NMR has gained great improvement in solving sensitivity problems and signal interferences by the eluents. Objective - Rapid analysis and characterisation by HPLC-SPE-NMR and LC/MS of the arylnaphthalene-type lignans present in Phyllanthus myrtifolius and the minor stilbenoids present in the polyphenol-rich fraction from the ethanol extract of the seeds of Syagrus romanzoffiana. Methodology - Pretreatment of fractions by liquid-liquid partitioning, followed by Sephadex LH-20 fractionation, was found very useful to facilitate the focusing and analysis of the polyphenolic fraction. HPLC-DAD-SPE-NMR (400 MHz and 600 MHz) analysis was carried out using an Agilent 1100 liquid chromatography, followed by a Prospekt 2 automated solid-phase extraction unit, containing 96 Hy Sphere-Resin GP cartridges (10 x 2 mm, 10-12 mu m), which was connected to a 120 or 60 mu L LC probe. Results - Seven arylnaphthalene-type lignans from the chloroform-soluble fraction of P. myrtifolius and nine stilbenoids from a polyphenol-rich butanol-soluble fraction of the seeds of S. romanzoffiana were characterised. Conclusion - HPLC-SPE-NMR associated with HR-ESI/MS, which consumed only analytical amounts of partially purified mixtures, was demonstrated to be a good tool for rapid screening of both known and new natural products. Copyright (C) 2011 John Wiley & Sons, Ltd.
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