On-line stop-flow two-dimensional liquid chromatography–mass spectrometry method for the separation and identification of triterpenoid saponins from ginseng extract
On-line stop-flow two-dimensional liquid chromatography–mass spectrometry method for the separation and identification of triterpenoid saponins from ginseng extract
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DOI：
10.1007/s00216-014-8219-4
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发表时间：
2014
影响因子：
4.3
通讯作者：
Shuangyuan Wang;Lizhen Qiao;Xianzhe Shi;Chunxiu Hu;Hongwei Kong;Guowang Xu
中科院分区：
文献类型：
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作者：
Shuangyuan Wang;Lizhen Qiao;Xianzhe Shi;Chunxiu Hu;Hongwei Kong;Guowang Xu
建立了停止流动二维液相色谱-电喷雾质谱联用（2D LC-ESI MS）分析人参主根三萜皂苷的方法。由于三萜皂苷的特殊结构（含有极性糖侧链和非极性苷元），分别采用亲水性相互作用色谱法（HILIC）和反相液相色谱法（RPLC）对其进行二维分析。一个陷阱柱被用来连接两个维度。在很大程度上避免了传统二维综合LC方法的主要缺点之一稀释效应。该系统的峰值容量为747，正交度为56.6%。与一维HILIC或RP - LC - MS分析相比，人参主要根提取物的质谱峰（强度大于1000的离子）分别增加了257和185%，并根据MS信息和总结的苷元结构鉴定出了94种三萜皂苷。该方法具有良好的线性和重复性，成功地应用于不同年龄（即生长年限）人参的分类，通过统计分析发现19种三萜皂苷的浓度随人参年龄的变化而变化。图解：用停止流动二维LC法分析皂苷的过程
A method based on stop-flow two-dimensional liquid chromatography coupled with electrospray ionization mass spectrometry (2D LC-ESI MS) was established and applied to analyze triterpenoid saponins from the main root of ginseng. Due to the special structure of triterpenoid saponins (they contain polar sugar side chains and nonpolar aglycones), hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RPLC) were used for the two dimensions, respectively. A trap column was used to connect the two dimensions. The dilution effect, which is one of the main shortcomings of traditional comprehensive 2D LC methods, was largely avoided. The peak capacity of this system was 747 and the orthogonality was 56.6 %. Compared with one-dimensional HILIC or RP LC MS analysis, 257 and 185 % more mass spectral peaks (ions with intensities that were higher than 1,000) were obtained from the ginseng main root extracts, and 94 triterpenoid saponins were identified based on MSninformation and summarized aglycone structures. Given its good linearity and repeatability, the established method was successfully applied to classify ginsengs of different ages (i.e., years of growth), and 19 triterpenoid saponins were found through statistical analysis to vary in concentration depending on the age of the ginseng.Graphical AbstractProcess of saponin's analysis using stop-flow 2D LC method