Abstract

Previously, we established a ¹H NMR metabolomics method using reversed-phase solid-phase extraction column (RP-SPEC), and succeeded in distinguishing wild from cultivated samples of Saposhnikoviae radix (SR), and between SR and its substitute, Peucedanum ledebourielloides root (PR). Herein, we performed LC-HR/MS metabolomics using fractions obtained via RP-SPEC to identify characteristic components of SR and PR. One and three characteristic components were respectively found for SR and PR; these components were isolated with their m/z values and retention times as a guide. The characteristic component of SR was identified as 4′-O-β-d-glucosyl-5-O-methylvisamminol (1), an indicator component used to identify SR in the Japanese Pharmacopoeia. In contrast, the characteristic components of PR were identified as xanthalin (2), 4′-O-β-d-apiosyl (1 → 6)-β-d-glucosyl-5-O-methylvisamminol (3), and 3′-O-β-d-apiosyl (1 → 6)-β-d-glucosylhamaudol (4) based on spectroscopic data such as 1D- and 2D-NMR, MS, and specific optical rotation. Among them, 4 is a novel compound. For the correlation between the NMR metabolomics results in the present and our previous report, only 1 and 2 were found to correlate with the chemical shifts, and the other compounds had no correlation. As the chemical shifts for compounds 1, 3, and 4 were similar to each other, especially for the aglycone moiety, they could not be distinguished because of the sensitivity and resolution of ¹H NMR. Accordingly, combining NMR and LC/MS metabolomics with their different advantages is considered useful for metabolomics of natural products. The series of methods used in our reports could aid in quality evaluations of natural products and surveying of marker components.

Graphic abstract

中文翻译：

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使用LC-HR / MS代谢组学鉴定可区分Saposhnikovia根及其替代物Peucedanum ledebourielloides根的化合物。

摘要

以前，我们使用反相固相萃取柱（RP-SPEC）建立了¹ H NMR代谢组学方法，并成功地将野生和人工培养的Saposhnikoviae radix（SR）样品以及SR及其替代物Peucedanum ledebourielloides根进行了区分。（PR）。本文中，我们使用通过RP-SPEC获得的馏分进行了LC-HR / MS代谢组学研究，以鉴定SR和PR的特征成分。SR和PR分别发现1个和3个特征成分。这些成分以其m / z值和保留时间为指导进行分离。SR的特征分量被确定为4'- ö -β- d -glucosyl -5- Ö -methylvisamminol（1），一种用于识别日本药典中SR的指标成分。与此相反，PR的特征分量被确定为xanthalin（2），4'- ö -β- d -apiosyl（1→6）-β- d -glucosyl -5- Ö -methylvisamminol（3），和3' -基于诸如1D-和2D-NMR，MS和比旋光度的光谱数据，O- β- d- apiosyl（1→6）-β- d-葡萄糖基hamaudol （4）。其中，4是新型化合物。对于当前和我们以前的报告中NMR代谢组学结果之间的相关性，只有1和2被发现与化学位移相关，而其他化合物则没有相关性。作为用于化合物的化学位移1，3，和4分别为彼此相似的，尤其是对糖苷配基部分，它们不能由于灵敏度和分辨率的区分¹ 1 H NMR。因此，将NMR和LC / MS代谢组学与它们的不同优点结合起来被认为对天然产物的代谢组学有用。我们报告中使用的一系列方法可以帮助评估天然产物的质量并调查标记物的成分。

图形摘要