[关键词]
[摘要]
目的 比较栀子炒制前后化学成分差异,明确其差异标志物,为栀子与炒栀子质量标准的制定提供参考。方法 采用全-精细指纹图谱和多指标含量同时测定对栀子炒制前后样品进行分析,采用层次聚类分析(HCA)、主成分分析(PCA)和正交偏最小二乘法-判别分析(OPLS-DA)等多元统计分析对栀子与炒栀子指纹图谱进行比较,筛选出导致差异的特征性成分。结果 栀子炒制前后指纹图谱中共有15个峰,其中12个峰为两者所共有,栀子与炒栀子对照指纹图谱的全指纹图谱相似度为0.991,而去除栀子苷积分后建立的精细指纹图谱相似度为0.880,低于0.90,可基本实现两者区分;多元统计分析结果表明栀子与炒栀子可明显分为2类,并筛选得到贡献度较大的4个差异标志物,分别为峰3、5、9(栀子苷)、11(西红花苷I);含量测定结果表明栀子炒制后栀子苷、西红花苷I、西红花苷II含量显著降低,而去乙酰车叶草酸甲酯含量显著升高。结论 栀子炒制前后成分差异显著,建立的精细指纹图谱结合多成分含量测定方法可有效区分栀子与炒栀子,筛选得到的差异标志物可为其质量标志物的选择提供参考。
[Key word]
[Abstract]
Objective To compare the differences of Gardeniae Fructus and its stir-baked preparation and screen out the differential markers, and provide reference for the establishment of quality standard. Methods The whole and partial fingerprints of Gardeniae Fructus and its stir-baked prepared slices were established by HPLC-UV analysis. And the fingerprints were statistically analyzed using hierarchical clustering analysis (HCA), principle component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA), then the characteristic markers were screened out. And then content of 6-α-hydroxygeniposide, gentioside, geniposide, crocin I, and crocin II was determined. Results A total of 15 peaks were acquired for Gardeniae Fructus and stir-baked Gardeniae Fructus respectively, 12 peaks of which were the common peaks. The similarity of whole and partial reference fingerprints of Gardeniae Fructus and its stir-baked prepared slices was 0.991 and 0.880, respectively, and partial fingerprint can successfully distinguished Gardeniae Fructus from its stir-baked prepared slices. HCA and OPLS-DA results showed that significant differences were observed between Gardeniae Fructus and stir-baked Gardeniae Fructus with peak 3, peak 5, peak 9 (geniposide), and peak 11 (crocin I), which being identified as the main differential markers. Contents of geniposide, crocin I and crocin II in Gardeniae Fructus were higher than those in stir-baked Gardeniae Fructus, while 6-α-hydroxygeniposide was lower. Conclusion The composition was significantly different before and after stir-baked. The established partial fingerprints combined with multi-component determination method can effectively distinguish them. And the differential markers obtained by multivariate statistical analysis can provide reference for the selection of quality markers.
[中图分类号]
R286.02
[基金项目]
国家中药标准化项目(ZYBZH-C-JS-33)