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目的:建立不同产地石上柏双黄酮的HPLC指纹图谱,并进行聚类分析和主成分分析,用于石上柏药材质量的评价。方法:采用Dikma Diamons C_(18)色谱柱(4.6 mm×150 mm,5μm),以乙腈-0.1%甲酸水溶液作为流动相,梯度洗脱,柱温25℃,流速0.6 mL·min~(-1),检测波长330 nm,进样量10μL。采用中药色谱指纹图谱相似度评价系统(2004A版)对10批样品进行共有峰确认及相似度评价。运用SPSS 17.0统计学软件对HPLC指纹图谱进行聚类分析和主成分分析。结果:方法学考察指标的相对标准偏差均<2.0%,表明在该色谱条件下,仪器精密度良好,样品在24 h内稳定性良好,方法准确度良好;根据10批药材测定结果表明,各共有峰较稳定,具有指纹图谱特征性,可初步拟定为石上柏双黄酮的指标成分群。在对照指纹图谱上共标定出9个色谱峰作为指纹图谱共有峰,指认了其中的3个化学成分,分别为穗花杉双黄酮、银杏双黄酮、扁柏双黄酮。10批样品的相似度计算结果均大于0.850,说明各产地的药材有较好的一致性;通过聚类分析可将10批样品可分为3类,第一类是重庆和四川产地的石上柏,第二类是贵州产地的石上柏,第三类是广西产地的石上柏,并且2个主成分的累计方差贡献率为98.096%。结论:该方法精密度高,重复性好,操作简便,可为石上柏药材的质量评价提供参考。
OBJECTIVE: To establish the HPLC fingerprints of bifendan in different habitats, and to conduct cluster analysis and principal component analysis to evaluate the quality of baihuashi. Methods: Dikma Diamons C_ (18) column (4.6 mm × 150 mm, 5 μm) was used with mobile phase of acetonitrile-0.1% formic acid as mobile phase and gradient elution. The column temperature was 25 ℃ and the flow rate was 0.6 mL · min -1 ), Detection wavelength 330 nm, injection volume 10μL. The chromatographic fingerprint similarity evaluation system (2004A version) was used to confirm the common peaks and evaluate the similarity of 10 batches of samples. Using the SPSS 17.0 statistical software, the fingerprint and principal component analysis of the HPLC fingerprints were analyzed. Results: The relative standard deviations (RSDs) were less than 2.0%, indicating that the precision of the instrument was good under the chromatographic conditions. The stability of the sample was good within 24 h and the accuracy of the method was good. According to the results of 10 batches of medicinal materials, The common peak is more stable and has the characteristic of fingerprinting, which can be initially formulated as the indicator component group of borax flavonoids. A total of 9 chromatographic peaks were identified on the control fingerprints as the common peaks of the fingerprints. Three chemical constituents were identified, namely biflavonoids, bilobalide and cypress flavone respectively. The similarity of 10 batches of samples was greater than 0.850, indicating that there is a good consistency of medicinal herbs in different producing areas. According to the cluster analysis, 10 batches of samples can be divided into three categories. The first category is ShiBai , The second one is ShiBaiBai from Guizhou origin, the third one is ShiBaiBai from Guangxi origin, and the cumulative contribution of two principal components is 98.096%. Conclusion: The method has high precision, good repeatability and simple operation, which can provide a reference for the quality evaluation of Radix.