微波辅助提取-高效液相色谱分析制备鸡骨草中相思子碱和下箴刺桐碱的研究

Analysis and Preparation of Abrine and Hypaphorine in Abrus Cantoniensis Based Upon Microwave-Assisted Extraction Coupled with High Performance Liquid Chromatography

建立了鸡骨草中相思子碱和下箴刺桐碱的微波辅助提取-高效液相色谱(MAE-HPLC)分析方法。优化得到的最佳微波辅助提取条件为:以25%甲醇为溶剂、固液比1:10(m/V)、提取温度50℃、提取时间10min。分析了广东、广西等7个不同产地鸡骨草中相思子碱和下箴刺桐碱含量,其中相思子碱含量范围0.03～0.84mg/g,回收率89.6%～92.9%,相对标准偏差(RSD)0.4%～3.9%;下箴刺桐碱含量范围0.06～0.62mg/g,回收率88.8%～95.5%,RSD 1.1%～3.4%。利用半制备高效液相色谱分离得到了相思子碱和下箴刺桐碱对照品,并采用电喷雾质谱(ESI-MS)和核磁共振(1H NMR)对其结构进行了表征。

A simple method based upon microwave-assisted extraction（MAE） coupled with high performance liquid chromatography for the analysis and preparation of abrine and hypaphorine in Abrus cantoniensis was developed.The optimal conditions for MAE were as follows：extraction solvent,25%（V/V） methanol;solid to liquid ratio,1：10;extraction temperature,50℃ and extraction time,10 min.The contents of abrine in Abrus cantoniensis from different habitats ranged from 0.03~0.84 mg/g,and the recoveries ranged from 89.6%~92.9% with RSD between 0.4%~3.9%;While the contents of hypaphorine ranged from 0.06~0.62 mg/g,and the recoveries were 88.8%~95.5% with RSD between 1.1%~3.4%.Abrine and hypaphorine were also prepared by semi-preparative high performance liquid chromatography,and their chemical structures were identified with ESI-MS and 1 H NMR.