HPLC-PDA-ELSD测定参芪五味子胶囊中10个成分含量及化学模式识别研究  

Simultaneous Determination of Ten Components in Shenqi Wuweizi Capsule by HPLC-PAD-ELSD Combined with Chemical Pattern Recognition

作　　者：赵娜[1] 付瑶 张诗航 张栋 张大方[2] ZHAO Na;FU Yao;ZHANG Shihang;ZHANG Dong;ZHANG Dafang(Changchun Humanities and Sciences College,Changchun 130117,China;Changchun University of Chinese Medicine,Changchun 130117,China)

机构地区：[1]长春人文学院,长春130117 [2]长春中医药大学,长春130117

出　　处：《中国现代应用药学》2021年第5期609-614,共6页Chinese Journal of Modern Applied Pharmacy

基　　金：吉林省科技发展计划项目(20170307003YY)。

摘　　要：目的建立HPLC-PDA-ELSD同时测定参芪五味子胶囊中毛蕊异黄酮葡萄糖苷、芒柄花苷、酸枣仁皂苷A、酸枣仁皂苷B、黄芪甲苷、党参炔苷、斯皮诺素、五味子酯甲、五味子酯乙、五味子甲素10个有效成分含量的方法,并结合主成分分析对其进行质量评价研究。方法样品采用70%甲醇提取后,采用Waters Symmetry C_(18)色谱柱(4.6 mm×250 mm,5μm)分离,流动相为含5%四氢呋喃的乙腈(A)-0.05%甲酸水溶液(B),梯度洗脱;流速为1.0 mL·min^(–1);柱温35℃;进样量10μL;毛蕊异黄酮葡萄糖苷、芒柄花苷、党参炔苷、斯皮诺素、五味子酯甲、五味子酯乙、五味子甲素检测波长:230 nm;酸枣仁皂苷A、酸枣仁皂苷B、黄芪甲苷使用ELSD检测器,漂移管温度60℃。并采用SIMCA14.1统计软件对含量测定结果进行主成分分析。结果在一定浓度范围内,参芪五味子胶囊中10个成分线性关系良好(r>0.999);平均加样回收率(n=9)为98.28%~102.95%,RSD均<2.0%。15批样品中毛蕊异黄酮葡萄糖苷、芒柄花苷、酸枣仁皂苷A、酸枣仁皂苷B、黄芪甲苷、党参炔苷、斯皮诺素、五味子酯甲、五味子酯乙、五味子甲素含量分别为0.136~0.152,0.296~0.323,0.334~0.403,0.074~0.114,2.401~2.504,1.455~1.512,0.094~0.164,2.031~2.214,0.711~0.809,1.892~1.973 mg·g^(–1)。主成分分析将参芪五味子胶囊分类为3类。结论所建立的HPLC-PDA-ELSD测定参芪五味子胶囊中10个成分含量方法快捷、准确、重复性好,专属性强,结合主成分分析法可为参芪五味子胶囊的质量控制提供参考。OBJECTIVE To develop an HPLC-PDA-ELSD method for the simultaneous determination of calycosin7-O-β-D-Glucopyranoside, ononin, jujuboside A, jujuboside B, astragaloside Ⅳ, lobetyolin, spinosin, schisantherin A, schisantherin B, deoxyschizandrin in Shenqi Wuweizi capsule, and to evaluate the quality of Shenqi Wuweizi capsule combined with principal component analysis. METHODS After the sample was extracted with 70% methanol, it was separated on a Waters Symmetry C18 column(4.6 mm×250 mm, 5 μm), and the mobile phase was acetonitrile(A) containing 5% tetrahydrofuran-0.05% formic acid aqueous solution(B) with gradient elution, the flow rate was 1.0 mL·min-1, and the column temperature was 35 ℃, the sample volume was 10 μL. Detection wavelength for calycosin7-O-β-D-glucopyranoside, ononin, lobetyolin, spinosin, schisantherin A, schisantherin B, deoxyschizandrin were set at 230 nm and ELSD was used for detection of jujuboside A, jujuboside B and astragaloside Ⅳ. The temperature of the drift tube was 60 ℃. The principal component analysis were conducted for the results of content determination by SIMCA14.1 statistical software. RESULTS Within a certain concentration range, the ten ingredients all showed good linear relationship(r>0.999), and the average recoveries were 98.28%-102.95% and RSDs were <2.0%. The contents of calycosin7-O-β-D-glucopyranoside, ononin, jujuboside A, jujuboside B, astragaloside Ⅳ, lobetyolin, spinosin, schisantherin A, schisantherin B, deoxyschizandrin in 15 samples were 0.136-0.152, 0.296-0.323, 0.334-0.403, 0.074-0.114, 2.401-2.504, 1.455-1.512, 0.094-0.164, 2.031-2.214, 0.711-0.809, 1.892-1.973 mg·g–1, respectively. The samples could be clearly classified into three categories by using PCA. CONCLUSION The established HPLC-PDA-ELSD method for the determination of 10 components in Shenqi Wuweizi capsule is fast, accurate, reproducible and specific, which can provide a reference for the quality control of Shenqi Wuweizi capsule combined with principal component analysis.

关 键 词：参芪五味子胶囊 高效液相色谱法 含量测定 模式识别 主成分分析 

分 类 号：R284.1[医药卫生—中药学]