基于HPLC-QAMS多指标成分定量测定联合化学计量学的津力达颗粒质量评价  

Quality Evaluation of Jinlida Granules(津力达颗粒)Based on HPLC-QAMS Multi-Index Quantitative Determination of Components Combined with Chemometrics

作　　者：王玉娟[1] 董玉波 孙莎莎 宁丽丽 任强[2] 周金辉[2] WANG Yu-juan;DONG Yu-bo;SUN Sha-sha;NING Li-li;REN Qiang;ZHOU Jin-hui(The 960^(th)Hospital of the Chinese People's Liberation Army,Ji'nan Shandong 250031,China;School of Pharmacy,Jining Medical College,Rizhao Shandong 276826,China)

机构地区：[1]中国人民解放军第960医院,山东济南250031 [2]济宁医学院药学院,山东日照276826

出　　处：《中医药导报》2022年第5期57-63,69,共8页Guiding Journal of Traditional Chinese Medicine and Pharmacy

基　　金：山东省中医药科技发展计划项目(2019-0449)。

摘　　要：目的:建立高效液相一测多评法定量测定津力达颗粒中人参皂苷Rb1、人参皂苷Rb3、人参皂苷Rd、3′-羟基葛根素、葛根素、3'-甲氧基葛根素、毛蕊花糖苷、焦地黄苯乙醇苷B1、苍术素醇、白术内酯Ⅱ和苍术素的含量,并结合化学计量学对产品质量进行综合评价。方法:以Waters HSST3 C18(250 mm×4.6 mm,5μm)为色谱柱,流动相为乙腈-0.2%磷酸,梯度洗脱,检测波长分别为203 nm(检测人参皂苷Rb1、人参皂苷Rb3、人参皂苷Rd)、254 nm(检测3′-羟基葛根素、葛根素、3'-甲氧基葛根素)和330 nm(检测毛蕊花糖苷、焦地黄苯乙醇苷B1、苍术素醇、白术内酯Ⅱ、苍术素)。以葛根素为内参物,建立其他10种成分的相对校正因子,并计算各成分含量。采用SPSS 26.0统计软件对津力达颗粒中11种成分含量测定结果进行聚类分析和主成分分析。结果:人参皂苷Rb1、人参皂苷Rb3、人参皂苷Rd、3′-羟基葛根素、葛根素、3'-甲氧基葛根素、毛蕊花糖苷、焦地黄苯乙醇苷B1、苍术素醇、白术内酯Ⅱ和苍术素分别在3.56~178.00、5.99~299.50、4.07~203.50、9.85~492.50、31.86~1593.00、7.58~379.00、2.15~107.50、0.86~43.00、0.59~29.50、1.47~73.50、2.69~134.50μg/mL范围内线性关系良好,相关系数(r)为0.9992~0.9997,平均加样回收率为96.77%~100.12%,RSD均<2.0%(n=9)。主成分分析和聚类分析结果一致,15批津力达颗粒聚为3类,主成分1~3是影响产品质量的主要因子。结论:所建立的高效液相一测多评法联合化学计量学可用于津力达颗粒中多指标性成分的定量测定和综合质量评价。Objective:To establish an HPLC-QAMS method for quantitative determination of ginsenoside Rb1,ginsenoside Rb3,ginsenoside Rd,3'-hydroxypuerarin,puerarin,3'-methoxypuerarin,verbascoside,Jionoside B1,atractylodinol,atractylodes lactone Ⅱ,atractydin in Jinlida Granules,and to comprehensively evaluate the product quality in combination with chemometrics.Methods:Waters HSST3 C_(18)(250 mm×4.6 mm,5μm)was used as the chromatographic column,and the mobile phase was acetonitrile-0.2% phosphoric acid with gradient elution.The detection wavelengths were 203 nm(detection of ginsenoside Rb1,ginsenoside Rb3,ginsenoside Rd),254 nm(detection of 3'-hydroxypuerarin,puerarin,3'-methoxypuerarin),and 330 nm(detection of verbascoside,Jionoside B1,atractylodinol,atractylodes lactone Ⅱ,atractydin),respectively.The relative correction factors of the other 10 components were established with puerarin as internal reference,and the contents of each component were calculated.Cluster analysis and principal component analysis were performed on the determination results of 11 components in Jinlida Granules by SPSS 26.0 statistical software.Results:The linear ranges of ginsenoside Rb1,ginsenoside Rb3,ginsenoside Rd,3'-hydroxypuerarin,puerarin,3'-methoxypuerarin,verbascoside,Jionoside B1,atractylodinol,atractylodes lactone Ⅱ,atractydin were 3.56-178.00,5.99-299.50,4.07-203.50,9.85-492.50,31.86-1593.00,7.58-379.00,2.15-107.50,0.86-43.00,0.59-29.50,1.47-73.50,2.69-134.50μg/mL,respectively.The correlation coefficient(r)was 0.9992-0.9997,the average recovery was 96.77%-100.12%,RSD<2.0%(n=9).The results of principal component analysis and cluster analysis were consistent,15 batches of Jinlida Granules were clustered into 3 categories,and principal components 1-3 were the main factors affecting product quality.Conclusion:The established HPLC-QAMS method combined with chemometrics method can be used for quantitative determination and comprehensive quality evaluation of multi-index components in Jinlida Granules.

关 键 词：津力达颗粒 高效液相一测多评法 多指标成分 化学计量学 相对校正因子 质量评价 主成分分析 聚类分析 

分 类 号：R284.2[医药卫生—中药学]