旋覆花配方颗粒HPLC特征图谱研究

Study on the Characteristic HPLC Chromatograms of Inula japonica Formula Granules

目的建立旋覆花配方颗粒HPLC特征图谱方法。方法采用高效液相色谱法,色谱柱为Agilent Zorbax Eclipse XDB-C_(18)(4.6 mm×250 mm,5μm),流动相为乙腈-0.1%磷酸溶液,梯度洗脱;流速为1.0m L·min^(-1);检测波长为230 nm;柱温为35℃;进样量为5μL。以绿原酸作为参照峰,测定13批旋覆花配方颗粒样品,建立对照特征图谱,并与同属其他植物花序制成的配方颗粒进行比较。结果建立了旋覆花配方颗粒的HPLC特征图谱,标定了11个特征峰,确定了其相对保留时间的范围,并对1,2,6,8,11号峰进行了指认。与旋覆花配方颗粒相比,地区习用品湖北旋覆花、水朝阳旋覆花、山黄菊配方颗粒图谱中虽然均可检测1~10号特征峰,但缺失11号旋覆花素特征峰,且3个品种制成配方颗粒较正品多检出12号去乙酰旋覆花素色谱峰。结论该方法稳定可靠,可用于旋复花配方颗粒的质量控制,并且可对不同植物来源制成的配方颗粒进行有效鉴别。

Objective To establish the characteristic HPLC chromatograms of Inula japonica formula granules.Methods HPLC was set up with Agilent Zorbax Eclipse XDB-C_（18） column, the mobile phase was comprised of acetonitrile（A） and 0.1% phosphoric acid, with a flow rate of 1.0 m L·min-1, detection wavelength of 230 nm,column temperature of 35 ℃,and sample volume of 5 μL. Using chlorogenic acid peak as reference,thirteen batches of Inula japonica formula granules were analyzed. Results Characteristic HPLC chromatogram was preliminarily established. Five characteristic peaks were confirmed and the fingerprints of different samples were compared by similarity evaluation software. Eleven chromatographic peaks were determined as common characteristic peaks of the HPLC characteristics. Chromatographic peak of inulicin were not found in formula granules of Inula hupehensis,Anisopappus chinensis or Inula helianthus-aquatica. Conclusion The established specific chromatogram with formula granules have high specificity and good repeatability, and can be used for multi-component qualitative analysis and quality control of Inula japonica formula granules.