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首页> 外文期刊>Electrophoresis: The Official Journal of the International Electrophoresis Society >Untargeted profiling of Glycyrrhiza glabra Glycyrrhiza glabra extract with comprehensive two‐dimensional liquid chromatography‐mass spectrometry using multi‐segmented shift gradients in the second dimension: Expanding the metabolic coverage
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Untargeted profiling of Glycyrrhiza glabra Glycyrrhiza glabra extract with comprehensive two‐dimensional liquid chromatography‐mass spectrometry using multi‐segmented shift gradients in the second dimension: Expanding the metabolic coverage

机译：用综合二维液相色谱 - 质谱法在第二层中的多分段移位梯度的综合二维液相色谱 - 质谱：扩大代谢覆盖率的综合二维液相色谱 - 质谱：未确定的二维液相色谱 - 质谱

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Abstract Metabolic profiling of Glycyrrhiza glabra using comprehensive two‐dimensional liquid chromatography (LC?×?LC) coupled with photodiode array (PDA) and mass spectrometry (MS) detection is described. The separation was conducted under reversed‐phase conditions, using a combination of first dimension ( 1 D) 150?mm microbore cyano column utilising 2.7 μm diameter ( d p ) particles, and second dimension ( 2 D) 50?mm superficially porous octadecylsilica column with 2.7?μm d p particles. A multi‐segmented shift gradient (MSG) for the 2 D separation was developed, and the orthogonality achieved was compared with other modes of gradients, such as full in‐fraction, and shift gradient systems. Results demonstrated a significant expansion of metabolic coverage using MSG in 2 D, providing the highest measure of orthogonality compared to other gradient modes. Compound identifications were performed by employing complementary data from PDA and MS detection, with reference to structural group‐type distribution in 2D space. A total of ca. 120 compounds were detected, and among them 37 were tentatively identified, distributed over the chemical families of glycosylated flavanones, triterpene saponins, and others. In comparison with one‐dimensional LC, the total number of compounds detected was ca. 2‐fold greater when LC?×?LC was employed. To the best of our knowledge, this is the first demonstration of the MSG mode in LC?×?LC, representing a powerful strategy to expand the metabolic coverage for analysis of plant‐derived extracts, containing a multitude of different phytochemical classes.
机译：摘要描述了使用综合二维液相色谱（LCα××LC）与光电二极管阵列（PDA）和质谱（MS）检测的综合二维液相色谱（LCα××LC）的代谢分析。利用2.7μm直径（DP）颗粒的第一尺寸（1d）150×mm微孔柱的组合，在反相条件下进行分离，使用2.7μm直径（dp）颗粒，第二尺寸（2d）50Ωmm，具有50Ωmm的半尺寸多孔的ondadecylsilica柱2.7？μmdp颗粒。开发了2d分离的多分段移位梯度（MSG），并将所达到的正交性与其他梯度模式进行比较，例如全部分馏，以及移位梯度系统。结果表明，使用MSG在2d中显着扩展了代谢覆盖率，与其他梯度模式相比，提供了最高的正交性度量。通过使用PDA和MS检测的互补数据，参考2D空间中的结构组型分布来进行复合鉴定。总共CA.检测到120种化合物，其中暂时鉴定出37，分布在糖基化的黄烷酮，三萜皂苷等化学品系上。与一维LC相比，检测到的化合物总数是Ca.当使用LC？××LC时更大2倍。据我们所知，这是LC？×ΔLC中MSG模式的第一次演示，代表强大的策略，以扩大用于分析植物衍生提取物的代谢覆盖，含有多种不同的植物化学类。

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