Abstract: Nuclear magnetic resonance/liquid chromatography-mass spectroscopy parallel dynamic spectroscopy (NMR/LC-MS PDS) is a method aimed at the simultaneous structural identification of natural products in complex mixtures. In this study, the method is illustrated with respect to 1H NMR and rapid resolution liquid chromatography-mass spectroscopy (RRLC-MS) data, acquired from the crude extract of Anoectochilus roxburghii, which was separated into a series of fractions with the concentration of constituent dynamic variation using reversed-phase preparative chromatography. Through fraction ranges and intensity changing profiles in 1H NMR/RRLC–MS PDS spectrum, 1H NMR and the extracted ion chromatogram (XIC) signals deriving from the same individual constituent, were correlated due to the signal amplitude co-variation resulting from the concentration variation of constituents in a series of incompletely separated fractions. 1H NMR/RRLC-MS PDS was then successfully used to identify three types of natural products, including eight flavonoids, four organic acids and p-hydroxybenzaldehyde, five of which have not previously been reported in Anoectochilus roxburghii. In addition, two groups of co-eluted compounds were successfully identified. The results prove that this approach should be of benefit in the unequivocal structural determination of a variety of classes of compounds from extremely complex mixtures, such as herbs and biological samples, which will lead to improved efficiency in the identification of new potential lead compounds.
Keywords: 1H NMR/RRLC-MS parallel dynamic spectroscopy; flavonoids; organic acids; crude extract; Anoectochilus roburghii
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Wang, X.-X.; He, J.-M.; Wang, C.-L.; Zhang, R.-P.; He, W.-Y.; Guo, S.-X.; Sun, R.-X.; Abliz, Z. Simultaneous Structural Identification of Natural Products in Fractions of Crude Extract of the Rare Endangered Plant Anoectochilus roxburghii Using 1H NMR/RRLC-MS Parallel Dynamic Spectroscopy. Int. J. Mol. Sci. 2011, 12, 2556-2571.
Wang X-X, He J-M, Wang C-L, Zhang R-P, He W-Y, Guo S-X, Sun R-X, Abliz Z. Simultaneous Structural Identification of Natural Products in Fractions of Crude Extract of the Rare Endangered Plant Anoectochilus roxburghii Using 1H NMR/RRLC-MS Parallel Dynamic Spectroscopy. International Journal of Molecular Sciences. 2011; 12(4):2556-2571.
Wang, Xiao-Xue; He, Jiu-Ming; Wang, Chun-Lan; Zhang, Rui-Ping; He, Wen-Yi; Guo, Shun-Xing; Sun, Rui-Xiang; Abliz, Zeper. 2011. "Simultaneous Structural Identification of Natural Products in Fractions of Crude Extract of the Rare Endangered Plant Anoectochilus roxburghii Using 1H NMR/RRLC-MS Parallel Dynamic Spectroscopy." Int. J. Mol. Sci. 12, no. 4: 2556-2571.