超临界流体色谱法分离丹参中亲脂性丹参酮。

IF 4 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS
Journal of Chromatography A Pub Date : 2025-10-11 Epub Date: 2025-08-06 DOI:10.1016/j.chroma.2025.466270
Donghai Xia, Chunying Song, Jing Feng, Dongping Yu, Yanfang Liu, Xinmiao Liang, Gaowa Jin, Zhimou Guo
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引用次数: 0

摘要

本研究系统地研究了亲脂性丹参酮(Tans)在不同固定相上的保留行为,并建立了在二元流动相(CO2和甲醇)下的超临界流体色谱(SFC)方法。非极性VCC18色谱柱对11种标准品的保留力极弱,几乎没有分离选择性。尽管使用几种典型的极性柱(Viridis Silica, Diol和NH2)和SFC专用柱(Torus 2-PIC)观察到一些改进,但峰的形状和选择性仍然很差。然而,高极性的Click TE-Cys色谱柱表现出良好的峰形,并实现了所有标准的完全分离,因此被确定为Tans的最佳固定相。这些结果表明,尽管tan具有亲脂性,但其保留主要受内部极性氧原子的影响,需要高极性柱而不是C18或传统极性柱来获得足够的分离选择性。此外,与RPLC相比,基于Click TE-Cys色谱柱的SFC分离方法具有更好的分离选择性和良好的正交性。通过离线SFC × RPLC-MS/MS分析证实了其应用潜力,在Tans中又标注了55个化合物,其中包括17个未知化合物。总的来说,本研究提供了含氧亲脂化合物在SFC中保留的机理见解,并为Tans分离提供了方法学上的进步,为类似化合物的SFC方法开发提供了理论基础。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Supercritical fluid chromatography for the separation of lipophilic tanshinones from Salvia miltiorrhiza Bunge.

This study systematically investigated the retention behavior of lipophilic tanshinones (Tans) on distinct stationary phases and developed a supercritical fluid chromatography (SFC) method under a binary mobile phase (CO2 and methanol). The non-polar VCC18 column showed extremely weak retention and virtually no separation selectivity for eleven standards. Despite some improvements observed with several typical polar columns (Viridis Silica, Diol, and NH2) and a SFC dedicated column (Torus 2-PIC), peak shapes and selectivity remained poor. However, a highly polar Click TE-Cys column exhibited good peak shapes and achieved complete separation of all standards, and was thus identified as the optimal stationary phase for Tans. These results indicate that despite the lipophilicity of Tans, their retention is primarily affected by internal polar oxygen atoms, requiring highly polar columns instead of C18 or conventional polar columns for adequate separation selectivity. In addition, the SFC separation method based on the Click TE-Cys column exhibited better separation selectivity and good orthogonality compared with RPLC. Its application potential was demonstrated by offline SFC × RPLC-MS/MS analysis, which annotated an additional 55 compounds in Tans, including 17 unknown compounds. Overall, this study provides mechanistic insights into the retention of oxygen-containing lipophilic compounds in SFC, as well as a methodological advance for Tans separation and a theoretical foundation for SFC method development of analogous compounds.

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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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