Ginsenoside Rg1의 NMR 데이터 동정

Abstract

수삼으로부터 용매추출, 용매분획 및 silica gel column chromatography를 반복하여 ginsenoside <TEX>$Rg_1$</TEX>을 분리하였다. Ginsenoside <TEX>$Rg_1$</TEX>의 결정특성, 녹는점, 비선광도, IR 데이터, FAB/MS 데이터, TLC에서의 Rf 값, HPLC에서의 r.t. 및 NMR 데이터를 표준화한 조건으로 측정하여 문헌 값과 비교 고찰하였다. 특히 ginsenoside <TEX>$Rg_1$</TEX>의 <TEX>$^{1}H-$</TEX> 및 <TEX>$^{13}C$</TEX>-NMR 데이터를 HSQC 및 HMBC와 같은 2D-NMR 실험을 통하여 정확하게 동정하였다. The fresh ginseng roots were extracted in aqueous methanol (MeOH), and the obtained extracts were partitioned using ethyl acetate (EtOA), n-butanol (n-BuOH), and water, successively. The repeated silica gel column chromatography for n-BuOH fraction afforded a purified ginsenoside <TEX>$Rg_1$</TEX>. The physico-chemical, spectroscopic and chromatographic data of ginsenoside <TEX>$Rg_1$</TEX>, such as crystallization characteristics, melting point, specific rotation, infrared spectrometry (IR) data, fast atom bombardment/mass spectrometry (FAB/MS) data, nuclear magnetic resonance (NMR) data, retention factor (Rf) in thin layer chromatography (TLC) experiment, and retention time (r.t.) in HPLC analysis, were measured and compared with those reported in literatures. Especially, the previous literatures reported different data for ginsenoside <TEX>$Rg_1$</TEX> in the <TEX>$^{1}H-$</TEX> and <TEX>$^{13}C$</TEX>-NMR experiments. This paper gives the exactly assigned NMR data through 2D-NMR experiments, such as <TEX>$^{1}H-^{1}H$</TEX> correlation spectroscopy (COSY), hetero nuclear single quantum correlation (HSQC), and hetero nuclear multiple bond connectivity (HMBC).