Nuclear magnetic resonance and liquid chromatography-mass spectrometry combined with an incompleted separation strategy for identifying the natural products in crude extract
Nuclear magnetic resonance and liquid chromatography-mass spectrometry combined with an incompleted separation strategy for identifying the natural products in crude extract
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核磁共振和液相色谱-质谱联用结合不完全分离策略鉴定粗提物中的天然产物
DOI：
10.1016/j.aca.2008.11.002
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发表时间：
2009-01-26
影响因子：
6.2
通讯作者：
Abliz, Zeper
中科院分区：
文献类型：
--
作者：
Dai, Dongmei;He, Jiuming;Abliz, Zeper
提出了NMR和LC-MS结合不完全分离的方法来同时鉴定粗提物中天然产物的结构，并建立了一种新的NMR/LC-MS平行动态光谱（NMR/LC-MS PDS）方法来发现保留时间（Rt）、通过对LC-MS和H-1 NMR并行可视化多光谱数据集的共同分析，得到了混合光谱中相同成分的质量/电荷（m/z）和化学位移（delta）数据。由于一系列不完全分离组分中各组分的浓度变化导致的信号幅值共变，从同一组分中提取的离子色谱（XIC）和H-1核磁共振信号在NMR/LC-MS PDS谱中通过分数范围和强度变化曲线相互关联。采用NMR/LC-MS PDS技术，对含黄酮醇苷类成分的中药活性提取物进行鉴定，并采用闪蒸柱色谱法将其分离成一系列组分。从混合光谱中同时发现了粗提物中同一成分的互补光谱信息。特别是，两组共洗脱异构体被成功鉴定。结果表明，NMR/LC-MS PDS结合不完全分离策略在离线模式下实现了与在线LC-NMR-MS分析相似的功能，具有简化和加速草药或其活性提取物成分结构鉴定的分析路线的潜力。(C) 2008 Elsevier B.V.版权所有
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 H-1 NMR. The extracted ion chromatogram (XIC) and H-1 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. (C) 2008 Elsevier B.V. All rights reserved.