采用高速逆流色谱和制备高效液相色谱从金银花花蕾中分离异绿原酸异构体。
Isolation of isochlorogenic acid isomers in flower buds of Lonicera japonica by high-speed counter-current chromatography and preparative high performance liquid chromatography.
机构信息
Taishan Scholar-Distinguished Experts Position, Key Disciplines on Analysis of Traditional Chinese Medicine, Shandong Key Laboratory of Chinese Medicine Quality Standard Research, Shandong Academy of Chinese Medicine, 7 West of Yanzishan Street, Jinan, Shandong 250014, China.
Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan, Shandong 250014, China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Feb 15;981-982:27-32. doi: 10.1016/j.jchromb.2014.12.020. Epub 2015 Jan 3.
An efficient method was established by HSCCC combined with prep-HPLC for separating isochlorogenic acid isomers from flower buds of Lonicera japonica. The partially purified sample from the methanol extract of flower buds of L. japonica by silica gel column was separated by HSCCC to result in a fraction containing two isochlorogenic acid isomers. The fraction was further isolated by prep-HPLC to yield isochlorogenic acid A and isochlorogenic acid C with purities of 98% and 96%, and the total recoveries at 80.1% and 79.8%, respectively. The chemical structures of isochlorogenic acid isomers were confirmed by electrospray ionization mass spectrometry (ESI-MS) and (1)H nuclear magnetic resonance (NMR).
建立了一种高效的 HSCCC 与半制备 HPLC 相结合的方法，用于从金银花花蕾中分离出绿原酸异构体。通过硅胶柱从金银花花蕾甲醇提取物中部分纯化的样品，通过 HSCCC 分离得到含有两种绿原酸异构体的馏分。该馏分进一步通过半制备 HPLC 分离，得到纯度分别为 98%和 96%的绿原酸 A 和绿原酸 C，总回收率分别为 80.1%和 79.8%。通过电喷雾电离质谱（ESI-MS）和（1）H 核磁共振（NMR）确定了绿原酸异构体的化学结构。
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