[关键词]
[摘要]
目的 采用HPLC指纹图谱法优化金银花物质组纯化工艺.方法 采用HPLC法建立金银花指纹图谱,以8种指标成分[新绿原酸、绿原酸、隐绿原酸、断马钱子苷半缩醛内酯(沃格闭花木苷)、木犀草苷、异绿原酸B、异绿原酸A和异绿原酸C]回收率和指纹图谱相似度为指标,优选大孔树脂型号、上样条件和洗脱条件.结果 XDA-8树脂对8个成分回收率最高.上样浓度为0.25 g/mL,pH值为3.5,上样量为0.9 g/g,4倍量40%和4倍量80%乙醇梯度洗脱,纯化后提取物8种成分的回收率为78%~96%,HPLC指纹图谱相似度大于0.98,成分均衡回收.结论 采用HPLC指纹图谱法优化金银花物质组大孔树脂纯化工艺,可保证纯化前后成分组成较高的一致性.
[Key word]
[Abstract]
Objective To optimize the technological parameters in the purification process of Lonicerae Japonicae Flos (LJF) materiomic with HPLC fingerprint technique. Methods Using the established HPLC fingerprint of LJF, the macroporous resin type, adsorption conditions, and elution requirements were optimized using the similarity and recovery rate of fingerprints of eight components (neochlorogenic acid, chlorogenic acid, cryptochlorogenin acid, vogeloside, luteoloside, isochlorogenic acid A, isochlorogenic acid B, and isochlorogenic acid C) as indexes. Results XDA-8 type resin possessed the highest recovery rates of eight components. The optimized purification process was as follows: The sample concentration was 0.25 g/mL, the ratio of sample to resin was 0.9 g/g, pH value was 3.5, and 40% ethanol (four times of resin volume) and 80% ethanol (four times of resin volume) were used as eluant, respectively. After being purified, the recovery rates of eight components were 78%—96%, and the similarity of fingerprint was higher than 0.98. These components could get balanced recovery. Conclusion Based on HPLC fingerprint technique, the optimized purification process of LJF materiomic with macroporous resin can ensure that the main components are consistent with the crude extract of LJF.
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[基金项目]
国家重点基础研究发展计划("973"计划)项目(2012CB724001);山东省自主创新专项(2013CXC20001)