半制备高效液相色谱制备5种苯乙醇苷类单体

Preparation of five phenylethanoid glycoside components by semi preparative HPLC

关键词:  半制备高效液相色谱  牛耳朵  苯乙醇苷类

Key words:  semi-preparative HPLC  Chirita eburnea  phenylethanoid glycosides

摘要:

利用MCI柱层析和半制备型反相高效液相色谱法从牛耳朵中分离制备了5种苯乙醇苷类单体。在Eclipse XDB C18(9.4 mm×250 mm,5 μm)半制备柱上,以甲醇 水为流动相,流速为4 mL/min,采用梯度洗脱方式,制备得到5个组分。经波谱(EI-MS,1H-NMR、13C-NMR)分析,分别鉴定为plantainoside(1)、chiritoside C(2)、plantaninoside B(3)、plantamajoside(4)和desrhamnosylverbascoside(5)。高效液相色谱分析表明所制备5种化合物纯度均高于98%。该方法分离条件简单,高效,一次可得到5个单体,目标产物纯度较高。

Abstract:

A method was established for the isolation and preparation of five phenylethanoid glycoside components from Chirita eburnea using MCI column chromatography and semi preparative HPLC. A semi preparative Eclipse XDB C18 (9.4 mm×250 mm,5 μm) was used in the preparation process. By gradient elution with methanol water as the mobile phase at a flow rate of 4 mL/min,five phenylethanoid glycoside components were obtained from Chirita eburnea,and on the basis of spectral data (EI-MS,1H-NMR,13C-NMR),these compounds were identified as plantainoside(1),chiritoside C(2),plantaninoside B(3),plantamajoside(4) and desrhamnosylverbascoside(5),and the purities of these five phenylethanoid glycoside components analyzed by HPLC were all beyond of 98%. The method is efficient,simple with high purification and got 5 components for one time.