山麦冬和麦冬皂苷类成分的HPLC/ESI-MS图谱研究

 目的鉴定山麦冬和麦冬中的皂苷成分,并建立其特征图谱。方法用甲醇提取山麦冬和麦冬对照药材,并用C₁₈SPE固相萃取柱除去提取液中的多糖成分制备供试液;用高效液相色谱-电喷雾离子阱质谱(HPLE/ESI-ITMS)研究供试液中的总皂苷成分并建立相应的特征图谱。实验条件为:AICHROM^TMRelizSilC₁₈(2.1mm×150mm,5μm)分析柱,流动相为10mmol·L^-1醋酸铵和乙腈(60min内乙腈浓度变化为25%～60%),流速为0.2mL·min^-1,自动进样后色谱分离、质谱检测。结果山麦冬、麦冬对照药材中分别有17个和14个特征色谱峰,根据各色谱峰的二级质谱碎片信息并参考有关文献,对其中的一些皂苷成分进行了初步定性分析。结论所测山麦冬与麦冬样品两者HPIE/ESI-ITMS的图谱特征性强,差异明显。

Characteristic fingerprints of saponins in Radix Liriopes and Radix Ophiopogonis by HPLC/ESI-MS

OBJECTIVE To identify the saponin components in Radix Liriopes and Radix Ophiopogonis and to develop their characteristic chromatograms by HPLC/ESI-MS. METHODS The saponins extracts from Radix Liriopes and Radix Ophiopogonis were determined by HPLC/ESI-MS. The separation was performed on a AICHROM^TM Reliz Sil C₁₈ column with the mobile phase consisting of ammonium acetate and acetonitrile in a gradient mode (acetonitrile changed from 25% to 60% in 60 min). The flow rate was 0.2 mL·min^-1. RESULTS Seventeen and fourteen chromatographic peaks of Radix Liriopes and Radix Ophiopogonis were separated and determined, respectively. The majority of saponins were identified by HPLC-MS/MS. CONCLUSION The characteristic chromatograms can be used to identify saponin components and for the quality control of Radix Liriopes and Radix Ophiopogonis.