[关键词]
[摘要]
目的 建立不同产地南柴胡Bupleurum scorzonerifolium多指标定量及质量差异评价方法。方法 采用UPLC-MS/MS法建立南柴胡药材中柴胡皂苷a、柴胡皂苷d、柴胡皂苷c、柴胡皂苷b2和柴胡皂苷f的含量测定方法,以乙腈-0.1%甲酸水溶液为流动相,体积流量0.3 mL/min,梯度洗脱,同时检测醇溶性浸出物、总灰分和酸不溶性灰分。采用SPSS 26.0和SIMCA 14.1软件对不同产地南柴胡样品进行聚类分析、主成分分析(principal component analysis,PCA)和正交偏最小二乘判别分析(orthogonal partial least squares discriminant analysis,OPLS-DA),结合变量重要性投影值(variable importance in projection,VIP)筛选影响南柴胡质量差异的标志性成分;采用CRITIC法对各评价指标进行客观赋权,并结合TOPSIS法构建南柴胡综合质量评价模型。结果 经方法学考察,各成分呈现良好的线性关系,准确度良好。定量分析结果显示不同产地南柴胡中5个化学成分含量分别为柴胡皂苷a(1.916±1.338)mg/g、柴胡皂苷c(0.753±0.445)mg/g、柴胡皂苷d(3.442±2.351)mg/g、柴胡皂苷b2(2.083±1.424)mg/g、柴胡皂苷f(0.463±0.322)mg/g,醇溶性浸出物、总灰分和酸不溶性灰分的量分别为(29.2±2.1)%、(6.0±0.6)%、(1.2±0.3)%;多元统计分析结果表明10批南柴胡明显分为2类,筛选出贡献度较大的3个质量差异标志物,按贡献度依次为柴胡皂苷d、柴胡皂苷b2和柴胡皂苷a;CRITIC-TOPSIS法分析结果显示样品产地为安徽毫州(S10)、甘肃陇南(S8)和甘肃定西(S5)的综合质量相对较好。结论 不同产地南柴胡药材质量存在差异。建立的多指标定量、化学计量学及CRITIC-TOPSIS法为完善南柴胡质量评价体系提供了实验依据。
[Key word]
[Abstract]
Objective To establish a method for multi-index quantitative analysis and quality difference evaluation of Bupleurum scorzonerifolium from different producing areas. Methods A UPLC-MS/MS method was developed for simultaneous determination of saikosaponin a, saikosaponin d, saikosaponin c, saikosaponin b2, and saikosaponin f in B. scorzonerifolium. The separation was performed with a mobile phase of acetonitrile-0.1% formic acid aqueous solution at a flow rate of 0.3 mL/min under gradient elution. Alcohol-soluble extractives, total ash, and acid-insoluble ash were also determined. Cluster analysis (CA), principal component analysis (PCA), and orthogonal partial least squares discriminant analysis (OPLS-DA) were conducted using SPSS 26.0 and SIMCA 14.1 software. The variable importance in projection (VIP) was used to identify markers contributing to quality differences. The CRITIC method was employed for objective weighting of each evaluation index, and a comprehensive quality assessment model was constructed by coupling with the TOPSIS method. Results Methodological validation results demonstrated good linearity and satisfactory accuracy for all analytes. The quantitative results showed that the contents of the five components in B. scorzonerifolium from different areas were: saikosaponin a (1.916 ± 1.338) mg/g, saikosaponin c (0.753 ± 0.445) mg/g, saikosaponin d (3.442 ± 2.351) mg/g, saikosaponin b2 (2.083 ± 1.424) mg/g, and saikosaponin f (0.463 ± 0.322) mg/g. The amounts of alcohol-soluble extractives, total ash, and acid-insoluble ash were (29.2 ± 2.1)%,( 6.0 ± 0.6)%, and (1.2 ± 0.3)%, respectively. Multivariate statistical analysis showed that the 10 batches of B. scorzonerifolium were clearly classified into two groups. Three quality difference markers with relatively high contribution were screened, and the order of contribution was saikosaponin d > saikosaponin b2 > saikosaponin a. The results of the CRITIC-TOPSIS analysis indicated that samples S10 (from Bozhou, Anhui), S8 (from Longnan, Gansu), and S5 (from Dingxi, Gansu) possessed relatively superior overall quality. Conclusion There are quality differences among B. scorzonerifolium samples from different producing areas. The established multi-index quantitative analysis, chemometrics, and CRITIC-TOPSIS method provide an experimental basis for improving the quality evaluation system of B. scorzonerifolium.
[中图分类号]
R282.6
[基金项目]
吉林省教育厅科学研究项目资助(JJKH20240653KJ)