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越婢加术汤的HPLC指纹图谱建立、含量测定及化学模式识别分析
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| 篇名： | 越婢加术汤的HPLC指纹图谱建立、含量测定及化学模式识别分析 |
| TITLE： | Establishment of HPLC Fingerprints ，Content Determination and Chemical Pattern Recognition Analysis of Yuebi Jiazhu Decoction |
| 摘要： | 目的：建立越婢加术汤的高效液相色谱（HPLC）指纹图谱，测定其中盐酸麻黄碱和盐酸伪麻黄碱的含量，同时进行化学模式识别分析。方法：以甘草酸铵为参照，使用《中药色谱指纹图谱相似度评价系统（2012版）》建立10批越婢加术汤的HPLC指纹图谱并进行相似度评价，结合混合对照品指认共有峰；采用HPLC法测定盐酸麻黄碱和盐酸伪麻黄碱的含量；采用SPSS26.0软件进行聚类分析，采用SIMCA13.0软件进行主成分分析和偏最小二乘法-判别分析，并筛选影响越婢加术汤质量的差异性成分。结果：越婢加术汤指纹图谱中共有20个共有峰，与对照指纹图谱的相似度均大于0.92；共指认了2个色谱峰，分别为甘草苷（峰11）和甘草酸铵（峰18）。盐酸麻黄碱、盐酸伪麻黄碱检测质量浓度的线性范围分别为0.98～48μg/mL（r＝0.9999）、1.02～51μg/mL（r＝0.9992）；精密度、重复性、稳定性（24h）试验的RSD均小于2％；平均加样回收率分别为105.67％（RSD＝2.88％，n＝9）、104.15％（RSD＝2.02％，n＝9）；含量分别为0.0081～0.0143、0.0025～0.0118mg/mL。聚类分析结果显示，10批越婢加术汤可聚为3类，S1聚为一类，S3聚为一类，S2、S4～S10聚为一类。主成分分析结果显示，S3位于得分图的最右侧，S1位于得分图的右侧，S2、S4～S10位于得分图的中部。偏最小二乘法-判别分析结果与聚类分析、主成分分析基本一致，且峰9、峰3、峰12、峰8、峰19、峰18（甘草酸铵）、峰13、峰20、峰11（甘草苷）的重要性投影值均大于1。结论：所建HPLC指纹图谱和含量测定方法操作简便、准确，结合化学模式识别可用于越婢加术汤的质量控制。峰9等9个成分为影响越婢加术汤质量的差异性成分。 |
| ABSTRACT： | OBJECTIVE：To establish the HPLC fingerprints of Yuebi jiazhu decoction ，determine the contents of ephedrine hydrochloride and pseudoephedrine hydrochloride and carry out chemical pattern recognition analysis. METHODS ：Using ammonium glycyrrhizinate as control ，HPLC fingerprint of 10 batches of Yuebi jiazhu decoction was established and the similarity was evaluated with Similarity Evaluation System for TCM Chromatographic Fingerprint （2012 edition），and common peaks were identified in combination with mixed control. HPLC method was used to determine the contents of ephedrine hydrochloride and pseudoephedrine hydrochloride. SPSS 26.0 software was used for cluster analysis ；SIMCA 13.0 software was used for principal component analysis and partial least squares discriminant analysis ；the differential components affecting the quality were screened. RESULTS：There were 20 common peaks in the fingerprint of Yuebi jiazhu decoction ，and the similarities with control fringerprint were all greater than 0.92. Two peaks were identified ，which were liquiritin （peak 11）and ammonium glycyrrhizate （peak 18）. The linear range of ephedrine hydrochloride and pseudoephedrine hydrochloride were 0.98-48 μg/mL（r＝0.999 9）and 1.02-51 μg/mL （r＝0.999 2），respectively. RSDs of precision ，reproducibility and stability tests （24 h）were all less than 2％. The average recoveries were 105.67％（RSD＝2.88％，n＝9）and 104.15％（RSD＝2.02％，n＝9），respectively. The contents of ephedrine hydrochloride and pseudoephedrine hydrochloride were 0.008 1-0.014 3，0.002 5-0.011 8 mg/mL. Results of cluster analysis showed that among the 10 batches of Yuebi jiazhu decoction ，S1 was clustered into one class ，S3 was clustered into one class ，and S2，S4-S10 were clustered into one class. The results of principal component analysis showed that S 3 was located at the far right side of the scoring plot ，S1 at the right side of the scoring plot ，and S 2，S4-S10 at the middle of the scoring plot. The results of partial least squares discriminant analysis were basically consistent with the results of cluster analysis and principal component analysis. The variable importance projection values of peak 9，peak 3，peak 12，peak 8，peak 19，peak 18 （ammonium glycyrrhizinate），peak 13，peak 20 and peak 11（liquiritin）were greater than 1. CONCLUSIONS ：Established HPLC fingerprint and the method for content determination are simple and accurate. Combined with chemical pattern recognition ，they can be used for the quality control of Yuebi jiazhu decoction. Nine components such as peak 9 are the differential components affecting the quality of Yuebi jiazhu decoction. |
| 期刊： | 2021年第32卷第22期 |
| 作者： | 赵峰，高太祥，石莉尧，王瑞 |
| AUTHORS： | ZHAO Feng，GAO Taixiang ，SHI Liyao，WANG Rui |
| 关键字： | 越婢加术汤；高效液相色谱法；指纹图谱；含量测定；化学模式识别 |
| KEYWORDS： | uebi jiazhu decoction ；HPLC；Fingerprint； |
| 阅读数： | 200 次 |
| 本月下载数： | 11 次 |
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