基于特征图谱、含量测定结合化学计量学分析的经典名方开心散质量评价研究

Study on Quality Evaluation of Famous Classical Formula Kaixin Powder Based on the Characteristic Chromatography， Content Determination Combined with Chemometrics Analysis

    摘要
  • 摘要:
    目的 建立开心散的特征图谱及多成分含量测定方法，结合相关化学计量学对多批次开心散进行质量评价。
    方法 采用HPLC-UV-ELSD联用法建立开心散特征图谱及多成分含量测定方法，采用主成分分析（Principal component analysis，PCA）对多批次开心散进行降维分析，同时采用Hotelling’s T2和DModX方法对不同批次开心散的质量设定控制范围。
    结果 15批开心散HPLC-UV特征图谱共确定26个特征峰并生成对照特征图谱，且与对照特征图谱比较相似度均>0.90；HPLC-ELSD特征图谱共确定18个特征峰，以人参皂苷Rb1为参照峰计算各特征峰相对保留时间，结果RSD为0.01%~0.39%，表明批间一致性较好。PCA分析得到表征开心散整体质量贡献较大的共有峰，其中远志酮Ⅲ、3，6′-二芥子酰基蔗糖、人参皂苷Re、Rb1为本研究含量测定指标。Hotelling’s T2和DModX控制上限分别为28.857、14.433和1.605、1.603。15批开心散中远志酮Ⅲ、3，6′-二芥子酰基蔗糖、β-细辛醚、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1含量分别为0.43~0.49、1.57~2.15、1.77~3.12、0.45~0.65、0.42~0.98、0.59~1.04 mg·g-1，线性关系良好（r≥0.998 1）；聚类热图分析结果表明，15批开心散可聚为2类。
    结论 建立的HPLC-UV-ELSD特征图谱和多成分含量测定方法简便准确，结合化学计量学可系统全面用于开心散的质量评价。拟定开心散HPLC-UV特征图谱相似度不低于0.90，HPLC-ELSD特征图谱下以人参皂苷Rb1为参照峰，15批开心散各特征峰相对保留时间平均值的±10%为限度，含量测定限度范围为远志酮Ⅲ 0.33~0.60 mg·g-1、3，6′-二芥子酰基蔗糖1.36~2.52 mg·g-1、β-细辛醚1.70~3.15 mg·g-1、人参皂苷Rg1+人参皂苷Re 0.80~1.48 mg·g-1、人参皂苷Rb1 0.56~1.04 mg·g-1。

     

    Abstract:
    OBJECTIVE To establish the characteristic chromatogram and multi-component content determination method of Kaixin Powder, and to evaluate the quality of multiple batches of Kaixin Powder using chemometric methods.
    METHODS The HPLC-UV-ELSD method was used to establish the characteristic chromatograms and multi-component content determination of Kaixin Powder, principal component analysis (PCA) was used for dimensionality reduction analysis of multiple batches of Kaixin Powder, and Hotelling’s T2 and DModX methods were used to set the quality control range of different batches of Kaixin Powder.
    RESULTS Fifteen batches of Kaixin Powder HPLC-UV characteristic chromatograms identified 26 characteristic peaks and generated a reference characteristic chromatogram, with a similarity greater than 0.90 compared to the reference characteristic chromatogram. HPLC-ELSD characteristic chromatograms identified 18 characteristic peaks, and the relative retention times of each characteristic peak were calculated based on ginsenoside Rb1 as a reference peak. The RSD was 0.01% to 0.39%, indicating good inter-batch consistency. PCA analysis identified common peaks that contribute significantly to the overall quality of Kaixin Powder, among which Polygalasaponin Ⅲ 3,6′-disinapoyl sucrose, Ginsenoside Re, and Rb1 were the indicators measured in this study. Hotelling’s T2 and DModX control limits were 28.857, 14.433 and 1.605, 1.603, respectively. The contents of polygalaxanthone Ⅲ, 3,6′-disinapoyl sucrose, β-asarone, ginsenoside Rg1, ginsenoside Re and ginsenoside Rb1 in 15 batches of Kaixin Powder were 0.43 to 0.49 mg·g-1, 1.57 to 2.15 mg·g-1, 1.77 to 3.12 mg·g-1, 0.45 to 0.65 mg·g-1, 0.42 to 0.98 mg·g-1, 0.59 to 1.04 mg·g-1, respectively, with good linear relationship (r≥0.998 1). The results of cluster heat map analysis showed that 15 batches of Kaixin Powder could be clustered into two categories.
    CONCLUSION The established HPLC-UV-ELSD characteristic chromatogram method and multi-component content determination method are convenient and accurate. Combined with chemometrics, they can be systematically and comprehensively used for the quality evaluation of Kaixin Powder. This study proposes that the HPLC-UV characteristic chromatogram similarity of Kaixin Powder should be no less than 0.90. Under the HPLC-ELSD characteristic chromatogram, ginsenoside Rb1 should be used as the reference peak, and the limit of the average relative retention time of each characteristic peak of 15 batches of Kaixin powder should be ±10%. The content determination limits should be as follows: Polygalasaponin III (0.33-0.60) mg·g-1, 3,6′-disinapoylsucrose (1.36-2.52) mg·g-1, β-asarone (1.70-3.15) mg·g-1, ginsenoside Rg1 + ginsenoside Re (0.80-1.48) mg·g-1, and ginsenoside Rb1 (0.56-1.04) mg·g-1.

     

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