[关键词]
[摘要]
目的 建立槲寄生黄酮类成分的特征指纹图谱,同时测定槲寄生中高圣草素-7-O-β-D-葡萄糖苷、高圣草素的含量,结合化学计量法分析,为其质量控制提供参考。方法 采用Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-0.1%磷酸溶液为流动相,梯度洗脱,体积流量1.0 mL·min-1,检测波长为285 nm,柱温30℃。建立14批槲寄生药材的黄酮类成分指纹图谱,结合化学计量学软件进行聚类分析(CA)、主成分分析(PCA)、偏最小二乘法-判别分析(PLS-DA)。在同一色谱条件下,经方法学验证,HPLC法同时测定14批槲寄生药材中高圣草素-7-O-β-D-葡萄糖苷、高圣草素。结果 建立了槲寄生药材黄酮类成分的指纹图谱,标定了7个共有特征峰,指认了其中2个峰:峰4 (高圣草素-7-O-β-D-葡萄糖苷)、峰6(高圣草素);其中12批槲寄生药材相似度达到0.9以上,聚类分析将14批样品分为2类;PCA分析共得到2个主成分,主成分1主要反映了特征峰2~7的信息,主成分2主要反映特征峰1的信息,峰4与峰6的峰面积较大,且对第1主成分的贡献也较大;PLS-DA结果表明,3个共有特征峰的变量重要性投影(VIP)值>1,依次为峰7、峰6、峰4。高圣草素-7-O-β-D-葡萄糖苷、高圣草素2个指标成分在一定质量浓度范围内线性关系良好,平均加样回收率分别为103.17%、101.47%,RSD分别为2.0%、0.7%,方法学考察结果均符合相关要求,14批样品中2种成分总质量分数为2.32~5.17 mg·g-1。结论 建立的方法准确、简便、重现性好,可为槲寄生药材的质量控制提供参考。
[Key word]
[Abstract]
Objective Under the same chromatographic conditions, establish a characteristic fingerprint of flavonoids in Viscum coloratum, and simultaneously determine the content of homoeriodictyol-7-O-β-D-glycoside and homoeriodictyol, combined with stoichiometric analysis, provides a reference for their quality control. Methods The separation was performed on a ZORBAX SB-C18 column (250 mm×4.6 mm, 5 μm) using a gradient elution with acetonitrile-0.1% phosphoric acid aqueous solution,and the flow rate at 1.0 mL·min-1,the detection wavelength at 285 nm,the column temperature was set at 30 ℃. The flavonoids fingerprints of 14 batches of Viscum coloratum were established, and cluster analysis (CA), principal component analysis (PCA), partial least squares discriminant analysis (PLS-DA) were performed with chemometrics software. Under the same chromatographic conditions, after being validated by formula, HPLC method was used to simultaneously determine the content of homoeriodictyol-7-O-β-D-glycoside and homoeriodictyol. Results The fingerprint of flavonoids in Viscum coloratum was established, seven common peaks were demarcated, and two of them were identified. The similarity of 12 batches of mistletoe was all above 0.9. Cluster analysis divided the 14 batches of samples into two categories. PCA analysis obtained a total of two principal components. Principal component 1 mainly reflects the information of feature peaks 2—7, while principal component 2 mainly reflects the information of feature peak 1. The peak areas of peaks 4 and 6 were larger, and their contribution to the first principal component were also significant. The PLSDA results indicate that the variable importance projection (VIP) values of the three common characteristic peaks are greater than 1, followed by peak 7, peak 6, and peak 4. The content derermination results showed that the two index components of homoeriodictyol-7-O-β-D-glycoside and homoeriodictyol had good linear relationship within a certain mass concentration range.The average recoveries were 103.17% and 101.47%, and the RSDs were 2.0% and 0.7% respectively. The results of content determination Methods met the relevant requirements, and the total content of two components in 14 batches of samples was 2.32— 5.17 mg·g-1. Conclusion The established method was accurate,simple and reproducible,which can provides an exprimental basis for the overall evaluation and quality control of Viscum coloratum.
[中图分类号]
R284.1
[基金项目]
寒地道地药材质量评价与开发利用关键技术研究及示范项目(GZ20210092)