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采用二维极性分离液相色谱-质谱联用技术对丹参中活性成分进行全面表征。

Comprehensive characterization of active components in Salvia miltiorrhiza using polarity-partitioned two-dimensional liquid chromatography coupled with mass spectrometry.

机构信息

School of Biology and Biological Engineering, South China University of Technology, Guangzhou 510006, PR China; Guangdong Institute of Food Inspection (Guangdong Inspection Center of Wine and Spirits), Guangzhou 510435, PR China.

School of Biology and Biological Engineering, South China University of Technology, Guangzhou 510006, PR China.

出版信息

J Chromatogr A. 2024 Nov 8;1736:465424. doi: 10.1016/j.chroma.2024.465424. Epub 2024 Oct 6.

DOI:10.1016/j.chroma.2024.465424
PMID:39405635
Abstract

Salvia miltiorrhiza, a widely used traditional Chinese medicine, contains a complex matrix of hydrophobic diterpenoids and hydrophilic phenolic acids, presenting significant challenges in comprehensive analysis. In this study, an online polarity-partitioned two-dimensional liquid chromatography coupled with mass spectrometry (2D-LC-MS) method was developed for comprehensive analysis of both lipophilic and hydrophilic active components in Salvia miltiorrhiza. The method integrated hydrophilic interaction liquid chromatography (HILIC) and reversed-phase liquid chromatography (RPLC), facilitating the efficient separation of compounds across a wide range of polarities. An online dilution strategy was implemented, minimizing sample loss and enhancing the method's utility for quality control and chemical characterization of complex herbal matrices. Compared with other LC methods, this approach significantly improved analyte coverage, resolution, and analysis efficiency. Under optimal conditions, 150 active components were successfully identified, including 33 compounds newly discovered in Salvia miltiorrhiza. Additionally, the validated online method was applied to the quantitative determination of 16 quality markers of Salvia miltiorrhiza from different sources. The results demonstrated the online method's potential as a superior alternative to existing techniques, offering broader applicability in traditional Chinese medicine research.

摘要

丹参是一种广泛使用的传统中药,含有复杂的疏水性二萜类和亲水性酚酸基质,在全面分析中存在重大挑战。本研究开发了一种在线极性分离二维液相色谱-质谱联用(2D-LC-MS)方法,用于全面分析丹参中的亲脂性和亲水性活性成分。该方法集成了亲水相互作用液相色谱(HILIC)和反相液相色谱(RPLC),能够有效分离广泛极性范围内的化合物。采用在线稀释策略,最大限度地减少了样品损失,提高了该方法在复杂草药基质的质量控制和化学特征分析中的实用性。与其他 LC 方法相比,该方法显著提高了分析物的覆盖率、分辨率和分析效率。在最佳条件下,成功鉴定了 150 种活性成分,包括在丹参中发现的 33 种新化合物。此外,还应用验证后的在线方法对来自不同来源的 16 种丹参质量标志物进行了定量测定。结果表明,该在线方法是现有技术的优越替代方法,在中药研究中具有更广泛的适用性。

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