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采用离心分配色谱法从[植物名称]变种中制备分离三种单萜类化合物。

Preparative Separation of Three Monoterpenes from var. Using Centrifugal Partition Chromatography.

作者信息

Nam Bomi, Paudel Sunil Babu, Kim Jin-Baek, Jin Chang Hyun, Lee Dongho, Nam Joo-Won, Han Ah-Reum

机构信息

Advanced Radiation Technology Institute, Korea Atomic Energy Research Institute, Jeongeup-si, Jeollabuk-do 56212, Republic of Korea.

College of Pharmacy, Yeungnam University, Gyeongsan-si, Gyeongsangbuk-do 38541, Republic of Korea.

出版信息

Int J Anal Chem. 2019 Jan 9;2019:8751345. doi: 10.1155/2019/8751345. eCollection 2019.

Abstract

Three monoterpenes, namely, 9-hydroxy isoegomaketone (), isoegomaketone (), and perilla ketone (), were successfully separated from the supercritical carbon dioxide (SC-CO) extract of the leaves of var. (cv. Antisperill; Lamiaceae) by centrifugal partition chromatography (CPC). To obtain large quantities of these materials required for studies on their mechanism of action and effectiveness in inflammation, we used CPC because of its high loading capacity and reproducibility to purify the three compounds. Compound (2.60 mg, 96.7% purity at 254 nm) was purified from 500 mg of the SC-CO extract of var. (cv. Antisperill), using a two-phase solvent system comprising -hexane/ethyl acetate/ethanol/water (5:5:5:5 v/v) in a descending mode. As compounds (56.1 mg, 97.6% purity at 254 nm) and (78.6 mg, 96.1% purity at 254 nm) are highly volatile and difficult to recover from an aqueous mobile phase after purification during the drying process, they were obtained from the same amount of the processed extract in an ascending mode using the upper organic phase as the mobile phase (-hexane/ethyl acetate/ethanol/water, 8:2:8:2 v/v). The structures of compounds - were confirmed by H- and C-NMR analysis. Thus, based on our findings, we recommend centrifugal partition chromatography as a powerful technique for purifying the active principal compounds and from the leaves of var. .

摘要

通过离心分配色谱法(CPC),从紫苏变种(cv. Antisperill;唇形科)叶片的超临界二氧化碳(SC-CO)提取物中成功分离出三种单萜类化合物,即9-羟基异莪术酮()、异莪术酮()和紫苏酮()。为了获得大量用于研究其作用机制和抗炎效果所需的这些物质,我们使用CPC,因为它具有高负载量和可重复性来纯化这三种化合物。使用包含正己烷/乙酸乙酯/乙醇/水(5:5:5:5 v/v)的两相溶剂系统,以下行模式从500 mg紫苏变种(cv. Antisperill)的SC-CO提取物中纯化出化合物(2.60 mg,在254 nm处纯度为96.7%)。由于化合物(56.1 mg,在254 nm处纯度为97.6%)和(78.6 mg,在254 nm处纯度为96.1%)具有高挥发性,并且在干燥过程中纯化后难以从水性流动相中回收,因此使用上层有机相作为流动相(正己烷/乙酸乙酯/乙醇/水,8:2:8:2 v/v),以上行模式从相同量的处理提取物中获得它们。通过氢核磁共振(H-NMR)和碳核磁共振(C-NMR)分析确定了化合物 - 的结构。因此,基于我们的研究结果,我们推荐离心分配色谱法作为从紫苏变种叶片中纯化活性主要化合物 和 的一种强大技术。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f84b/6343183/f2283c523290/IJAC2019-8751345.001.jpg

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