高效液相色谱法同时测定景天祛斑胶囊中10种成分含量

Simultaneous Determination of Ten Compositions in Jingtian Quban Capsules by HPLC

目的建立高效液相色谱(HPLC)法同时测定景天祛斑胶囊中毛蕊异黄酮葡萄糖苷、芒柄花苷、9,10-二甲氧基紫檀烷-3-O-β-D-葡萄糖苷、毛蕊异黄酮、红景天欧素、红景天宁、大花红景天素、阿魏酸松柏酯、藁本内酯和欧当归内酯含量,采用化学计量学方法对检测结果进行综合评价。方法以乙腈-0.2%甲酸为流动相;采用Agilent ZORBAX SB-C_(18)(4.6 mm×250 mm,5μm)色谱柱,柱温30℃;检测波长分别为254 nm(检测毛蕊异黄酮葡萄糖苷、芒柄花苷、9,10-二甲氧基紫檀烷-3-O-β-D-葡萄糖苷和毛蕊异黄酮)、382 nm(检测红景天欧素、红景天宁和大花红景天素)和280 nm(检测阿魏酸松柏酯、藁本内酯和欧当归内酯);流量:0.9 mL·min^(-1)。采用SPSS 26.0版统计软件对景天祛斑胶囊中10种成分含量测定结果进行聚类分析和主成分分析。结果毛蕊异黄酮葡萄糖苷、芒柄花苷、9,10-二甲氧基紫檀烷-3-O-β-D-葡萄糖苷、毛蕊异黄酮、红景天欧素、红景天宁、大花红景天素、阿魏酸松柏酯、藁本内酯和欧当归内酯分别在4.18~167.20,2.49~99.60,3.07~122.80,1.81~72.40,5.69~227.60,3.46~138.40,0.58~23.20,8.77~350.80,6.59~263.60,0.86~34.40μg·mL^(-1)范围内线性关系良好;平均加样回收率分别为98.44%,97.87%,99.20%,96.95%,99.54%,100.09%,96.99%,99.72%,100.03%和97.74%,RSD分别为1.30%,1.51%,1.05%,0.98%,0.87%,0.72%,1.26%,0.86%,0.67%和1.18%;10批样品聚类分析为3类;主成分1—4是影响景天祛斑胶囊质量评价的重要因子。结论该方法准确、可靠,可用于景天祛斑胶囊多指标质量评价。

Objective To establish a high-performance liquid chromatography(HPLC)method for simultaneous determination of calycosin-7-glucoside,ononin,9,10-dimethoxy-pterocarpane-3-O-β-D-glucoside,calycosin,rhodiosin,rhodionin,rhodiolin,coniferyl ferulate,ligustilide and levistilide A in Jingtian quban capsules,and combine chemometrics to comprehensive evaluate the quality of Jingtian quban capsules.Methods The separation was performed by HPLC equipped with an Agilent ZORBAX SB-C_(18) chromatographic column.The mobile phase consisted of acetonitrile-0.2%formic acid in a gradient elution method.The column temperature was set at 30℃,and the flow rate was 0.9 mL·min^(-1).The detection wavelength were set at 254 nm for calycosin-7-glucoside,ononin,9,10-dimethoxy-pterocarpane-3-O-β-D-glucoside and calycosin,382 nm for rhodiosin,rhodionin and rhodiolin,and 280 nm for coniferyl ferulate,ligustilide and levistilide A.The cluster analysis and principal component analysis were conducted for the content results of ten constituents in Jingtian quban capsules by SPSS 26.0 statistical software.Results A good linear relationship was observed within the range of 4.18-167.20μg·mL^(-1) for calycosin-7-O-β-D-glucoside,2.49-99.60μg·mL^(-1) for ononin,3.07-122.80μg·mL^(-1) for 9,10-dimethoxy-pterocarpane-3-O-β-D-glucoside,1.81-72.40μg·mL^(-1) for calycosin,5.69-227.60μg·mL^(-1) for rhodiosin,3.46-138.40μg·mL^(-1) for rhodionin,0.58-23.20μg·mL^(-1) for rhodiolin,8.77-350.80μg·mL^(-1) for coniferyl ferulate,6.59-263.60μg·mL^(-1) for ligustilide and 0.86-34.40μg·mL^(-1) for levistilide A.The average recovery rates of each detected component of Jingtian quban capsules were 98.44%,97.87%,99.20%,96.95%,99.54%,100.09%,96.99%,99.72%,100.03%and 97.74%with the RSDs of 1.30%,1.51%,1.05%,0.98%,0.87%,0.72%,1.26%,0.86%,0.67%and 1.18%,respectively.The samples of 10 batches of Jingtian quban capsules could be divided in to 3 categories.The principal components 1-4 were the main factors affecting Jingtian quban capsules quality evaluation.Conclusion The method is accurate and reliable,and can be used to evaluate the quality of Jingtian quban capsules.