Record number :
Title of article :
Nuclear magnetic resonance and liquid chromatography–mass spectrometry combined with an incompleted separation strategy for identifying the natural products in crude extract Original Research Article
Author/Authors :
Dongmei Dai، نويسنده , , Jiuming Zhang، نويسنده , , Ruixiang Sun، نويسنده , , Ruiping Zhang، نويسنده , , Haji Akber Aisa، نويسنده , , Zeper Abliz، نويسنده ,
Issue Information :
روزنامه با شماره پیاپی سال 2009
Pages :
From page :
To page :
Abstract :
NMR and LC–MS combined with an incompleted separation strategy were proposed to the simultaneous structure identification of natural products in crude extracts, and a novel method termed as NMR/LC–MS parallel dynamic spectroscopy (NMR/LC–MS PDS) was developed to discover the intrinsic correlation between retention time (Rt), mass/charge (m/z) and chemical shift (δ) data of the same constituent from mixture spectra by the co-analysis of parallelly visualized multispectroscopic datasets from LC–MS and 1H NMR. The extracted ion chromatogram (XIC) and 1H NMR signals deriving from the same individual constituent were correlated through fraction ranges and intensity changing profiles in NMR/LC–MS PDS spectrum due to the signal amplitude co-variation resulted from the concentration variation of constituents in a series of incompletely separated fractions. NMR/LC–MS PDS was applied to identify 12 constituents in an active herbal extract including flavonol glycosides, which was separated into a series of fractions by flash column chromatography. The complementary spectral information of the same individual constituent in the crude extract was discovered simultaneously from mixture spectra. Especially, two groups of co-eluted isomers were identified successfully. The results demonstrated that NMR/LC–MS PDS combined with the incompleted separation strategy achieved the similar function of on-line LC–NMR–MS analysis in off-line mode and had the potential for simplifying and accelerating the analytical routes for structure identification of constituents in herbs or their active extracts.
Keywords :
Nuclear magnetic resonance/liquid chromatography–mass spectrometry parallel dynamic spectroscopy , Incompleted separation strategy , Off-line analytical method , Crude extract , Natural products
Journal title :
Analytica Chimica Acta
Link To Document :