基于指纹图谱及多指标成分定量结合化学计量法的跌打祛风膏质量评价OA
Quality Evaluation of Dieda Qufeng Plaster Based on HPLC Fingerprint Profiling,Multi-Index Component Quantification and Chemometrics
目的 建立跌打祛风膏的高效液相色谱(HPLC)指纹图谱,测定其 8 种成分含量,并结合化学计量法综合评价跌打祛风膏的质量.方法 采用岛津Shim-pack GIST C18-AQ色谱柱(4.6 mm×250 mm,5 μm),以乙腈-0.05%磷酸水为流动相梯度洗脱,波长 206 nm,柱温 30℃,进样量 10 μL,流速 1.0 mL·min-1,构建10 批跌打祛风膏的HPLC指纹图谱;同时测定其 8 种成分(香草醛、阿魏酸、柚皮苷、苯甲酸、羌活醇、蛇床子素、大黄素和异欧前胡素)的含量,并采用聚类分析(HCA)、主成分分析(PCA)和正交偏最小二乘法判别分析(OPLS-DA)综合评价 10 批跌打祛风膏的质量.结果 10 批跌打祛风膏HPLC指纹图谱共确定 29 个共有峰,相似度均＞0.950.10 批跌打祛风膏中香草醛、阿魏酸、柚皮苷、苯甲酸、羌活醇、蛇床子素、大黄素和异欧前胡素的含量分别为 26.071 4～77.457 8、2.657 7～12.982 0、5.368 5～19.502 4、101.082 7～453.386 0、15.024 0～57.219 1、2.228 9～22.676 8、28.187 1～41.741 4、18.775 8～51.405 7 μg·g-1.HCA分析结果显示,10 批跌打祛风膏可分为S1、S2～S4、S5～S7、S8～S10 四类;PCA得到 5 个主成分的累积方差贡献率为94.314%;OPLS-DA筛选出 8 个成分[峰 5、峰 9、峰 13、峰 14(苯甲酸)、峰 19、峰 22、峰 26(异欧前胡素)、峰 29]是影响跌打祛风膏质量的差异质量标志物.结论 该研究建立的HPLC指纹图谱及多指标成分测量方法稳定、可靠,可为跌打祛风膏的质量控制提供科学依据.
Objective To establish a high-performance liquid chromatography(HPLC)fingerprint for Dieda Qufeng Plaster,simultaneously determine the contents of eight characteristic components,and comprehensively evaluate its quality by combining chemometric methods.Methods An HPLC fingerprint method for 10 batches of Dieda Qufeng Plaster was developed using a Shimadzu Shim-pack GIST C18-AQ column(4.6 mm×250 mm,5 μm).The mobile phase consisted of acetonitrile and-0.05%phosphoric acid aqueous solution with gradient elution.The detection wavelength was set at 206 nm,the column temperature at 30℃,the injection volume at 10 μL,and the flow rate at 1.0 mL·min-1.Simultaneously,the contents of eight components-vanillin,ferulic acid,naringin,benzoic acid,notopterol,osthole,emodin,and isoimperatorin were determined.The quality of the 10 batches was comprehensively evaluated using hierarchical cluster analysis(HCA),principal component analysis(PCA),and orthogonal partial least squares-discriminant analysis(OPLS-DA).Results The HPLC fingerprints of the 10 batches identified 29 common peaks,with similarity values all exceeding 0.950.The content ranges for the eight components were as follows:vanillin 26.071 4-77.457 8 μg·g-1,ferulic acid 2.657 7-12.982 0 μg·g-1,naringin 5.368 5-19.502 4 μg·g-1,benzoic acid 101.082 7-453.386 0 μg·g-1,notopterol 15.024 0-57.219 1 μg·g-1,osthole 2.228 9-22.676 8 μg·g-1,emodin 28.187 1-41.741 4 μg·g-1,and isoimperatorin 18.775 8-51.405 7 μg·g-1.HCA results showed that the 10 batches could be classified into four categories:S1,S2-S4,S5-S7,and S8-S10.PCA yielded five principal components with a cumulative variance contribution rate of 94.314%.OPLS-DA identified eight components[peak 5,peak 9,peak 13,peak 14(benzoic acid),peak 19,peak 22,peak 26(isoimperatorin),and peak 29]as differential quality markers affecting the quality of Dieda Qufeng Plaster.Conclusion The established HPLC fingerprint method combined with multi-index component quantification is stable and reliable,providing a scientific basis for the quality control of Dieda Qufeng Plaster.
莫静媛;黄小玲;谢询;黄晓晴;苏安宇;黄晓冰;黄雨威;王利胜
广州中医药大学中药学院,广东 广州 510006广州中医药大学中药学院,广东 广州 510006广州中医药大学中药学院,广东 广州 510006广州中医药大学中药学院,广东 广州 510006东莞市中医院,广东 东莞 523005广州中医药大学第三附属医院,广东 广州 510378武汉市中医院,湖北 武汉 430014广州中医药大学中药学院,广东 广州 510006
医药卫生
跌打祛风膏指纹图谱含量测定化学计量法差异质量标志物
Dieda Qufeng Plasterfingerprintcontent determinationchemometricsdifferential quality markers
《中药新药与临床药理》 2026 (1)
169-178,10
湖北省武汉市医学科研项目(WZ19C29)广州市科技计划项目(2022060188)广东省基础与应用基础研究项目(2022A1515220078).
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