Identification of the major constituents of Hypericum perforatum by LC/SPE/NMR and/or LC/MS

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• 作者：Evangelos C. Tatsis ; Sjef Boeren ; Vassiliki Exarchou ; Anastassios N. Troganis ; Jacques Vervoort ; Ioannis P. Gerothanassis
• 关键词：Hypericum perforatum ; LC/SPE/NMR ; Dereplication ; Hyperforin ; Hyperfirin ; Flavonoids
• 刊名：Phytochemistry
• 出版年：2007
• 出版时间：February 2007
• 年：2007
• 卷：68
• 期：3
• 页码：383-393
• 全文大小：527 K

文摘

The newly established hyphenated instrumentation of LC/DAD/SPE/NMR and LC/UV/(ESI)MS techniques have been applied for separation and structure verification of the major known constituents present in Greek Hypericum perforatum extracts. The chromatographic separation was performed on a C18 column. Acetonitrile-water was used as a mobile phase. For the on-line NMR detection, the analytes eluted from column were trapped one by one onto separate SPE cartridges, and hereafter transported into the NMR flow-cell. LC/DAD/SPE/NMR and LC/UV/MS allowed the characterization of constituents of Greek H. perforatum, mainly naphtodianthrones (hypericin, pseudohypericin, protohypericin, protopseudohypericin), phloroglucinols (hyperforin, adhyperforin), flavonoids (quercetin, quercitrin, isoquercitrin, hyperoside, astilbin, miquelianin, I3,II8-biapigenin) and phenolic acids (chlorogenic acid, 3-O-coumaroylquinic acid). Two phloroglucinols (hyperfirin and adhyperfirin) were detected for the first time, which have been previously reported to be precursors in the biosynthesis of hyperforin and adhyperforin.