title: Nuclear magnetic resonance and liquid chromatography-mass spectrometry combined with an incompleted separation strategy for identifying the natural products in crude extract.
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 (delta) data of the same constituent from mixture spectra by the co-analysis of parallelly visualized multispectroscopic datasets from LC-MS and (1)H NMR. The extracted ion chromatogram (XIC) and (1)H 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.
authors.affiliation: Key Laboratory of Bioactive Substances and Resource Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing, China.
authors.forename: Dongmei
authors.initials: D
authors.lastname: Dai
authors.forename: Jiuming
authors.initials: J
authors.lastname: He
authors.forename: Ruixiang
authors.initials: R
authors.lastname: Sun
authors.forename: Ruiping
authors.initials: R
authors.lastname: Zhang
authors.forename: Haji Akber
authors.initials: HA
authors.lastname: Aisa
authors.forename: Zeper
authors.initials: Z
authors.lastname: Abliz
mesh_terms: D001688:Biological Products / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D045424:Complex Mixtures / Q000737:chemistry*; D003368:Gossypium / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D010936:Plant Extracts / Q000737:chemistry; D013997:Time Factors
chemical_list: D001688:Biological Products; D045424:Complex Mixtures; D010936:Plant Extracts