UPLC-PDA同时测定肝复康丸中10个成分含量及主成分分析

Simultaneous Determination of Nine Components in Ganfukang Pills by UPLC-PDA

目的:建立超高效液相色谱法(UPLC)同时测定肝复康丸中芦丁、齐墩果酸、槲皮素、太子参环肽B、山柰酚、熊果酸、五味子醇甲、五味子酯甲、五味子甲素、五味子乙素10个成分含量的方法。方法:采用Agilent Ecilipse C 18色谱柱(100 mm×2.1 mm,1.6μm),流动相为乙腈-0.05%磷酸水溶液,梯度洗脱;流速为0.3 mL·min^(-1);检测波长分别为203、210、360 nm;柱温为30℃;采用SPSS 22.0统计软件对含量测定结果进行主成分分析与聚类分析。结果:在一定质量浓度范围内,肝复康丸中10个成分均呈良好的线性关系(r>0.999);平均加样回收率为97.9%~104.9%(RSD<1.5%),13批样品中芦丁、齐墩果酸、槲皮素、太子参环肽B、山柰酚、熊果酸、五味子醇甲、五味子酯甲、五味子甲素、五味子乙素质量分数分别为1.104~1.499、1.463~1.707、0.861~1.223、0.596~0.921、0.754~0.923、2.594~2.966、3.716~3.797、2.204~2.336、0.963~1.369、0.782~1.052 mg·g^(-1)。聚类分析将不同生产厂家的肝复康丸分为3类,经主成分分析,C厂家的样品综合得分最高。结论:经方法学验证,本法可用于肝复康丸的质量控制。

Objective:To develop an ultra-performance liquid chromatography with photodiode array(UPLC-PDA)method for simultaneous determination of the 10 components in Ganfukang Pills:rutin,oleanolic acid,quercetin,heterophyllin B,kaempferol,ursolic acid,schisandrin,schisantherin A,deoxyschizandrin,and γ-schisandrin.Methods:UPLC conditions are as below:Agilent Ecilipse C 18 Column(100 mm×2.1 mm,1.6μm),mobile phase of acetonitrile-0.05%phosphoric acid solution with gradient elution at the flow rate of 0.3 mL·min^(-1),detection wavelengths of 203,210,360 nm,column temperature of 30℃.SPSS 22.0 was employed for principal component analysis(PCA)and cluster analysis(CA)of content determination results.Results:Within certain concentration ranges,the 10 components all showed good linear relationships(r>0.999)and the average recoveries were in the range of 97.9%-104.9%(RSD<1.5%).The content of rutin,oleanolic acid,quercetin,heterophyllin B,kaempferol,ursolic acid,schisandrin,schisantherin A,deoxyschizandrin,γ-schisandrin in 13 samples was 0.104-1.499,1.463-1.707,0.861-1.223,0.596-0.921,0.754-0.923,2.594-2.966,3.716-3.797,2.204-2.336,0.963-1.369,and 0.782-1.052 mg·g^(-1),respectively.The samples were classified into three clades by CA.According to the PCA result,products of manufacturer C had the highest quality.Conclusion:The established method can be used for the quality control of Ganfukang Pills.