女珍颗粒中4种成分的含量测定及其主成分分析和聚类分析

Content Determination,Principal Component Analysis and Cluster Analysis of Four Constituents in Nvzhen Granules

目的:建立UPLC-MS/MS法同时测定女珍颗粒中红景天苷、女贞苷、特女贞苷和蟛蜞菊内酯含量的方法。方法:样品经甲醇超声提取后,采用Agilent SB-C_(18)色谱柱(100 mm×2.1 mm,1.8μm),乙腈(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱,体积流量0.3 ml·min^(-1),柱温40℃,进样量1μl,采用电喷雾正离子源,多反应监测进行定量测定,测定结果采用SPSS 20.0软件进行聚类分析和主成分分析。结果:10批样品中各成分色谱峰分离良好,红景天苷、女贞苷、特女贞苷和蟛蜞菊内酯分别在2.434~121.72 ng(r=0.9987)、3.127~156.33 ng(r=0.9997)、4.624~231.20 ng(r=0.9993)和1.883~94.15 ng(r=0.9992)范围内线性关系良好;平均回收率分别为96.63%,98.53%,100.70%,95.31%,RSD分别为1.30%,1.59%,1.10%,3.25%(n=6)。10批样品聚为2大类,主成分1累计贡献率达到71.345%。结论:所建立的方法灵敏、快速、准确,可用于女珍颗粒的质量控制。

Objective:To develop a UPLC-MS/MS method for the simultaneous determination of salidroside,ligustroflavone,specnuezhenide and wedelolactone in Nvzhen granules.Methods:The samples were extracted by methanol and separated on an Agilent SB-C_(18) column(100 mm×2.1 mm,1.7μm)with mobile phase consisting of acetonitrile-0.1%formic acid in a gradient elution mode.The flow rate was 0.3 ml·min^(-1),the column temperature was 40℃and the volume of injection was 1μl.Multiple-reaction monitoring scanning was used for quantification with electrospray positive ions model.The data were used for principal component analysis(PCA)and cluster analysis(CA)by SPSS 20.0 software.Results:The chromatographic peak of each component in ten batches were well separated.The linear ranges of salidroside,ligustroflavone,specnuezhenide and wedelolactone were 2.434-127.72 ng(r=0.9987),3.127-156.33 ng(r=0.9997),4.624-231.20 ng(r=0.9993)and 1.883-94.15 ng(r=0.9992),respectively.The average recoveries were 96.63%,98.53%,100.70%and 95.31%with the RSDs of 1.30%,1.59%,1.10%and 3.25%(n=6),respectively.Ten batches of samples were divided into two categories and the cumulative contribution rate of the first principal component was 71.345%.Conclusion:The established method is rapid,sensitive and accurate,which can be used for the quality control of Nvzhen granules.