[关键词]
[摘要]
目的 建立黑龙骨Periploca forrestii茎叶(PFSL)中7个成分的UPLC测定方法 ,并对结果进行化学计量学分析。方法采用Agilent Eclipse Plus C18色谱柱(100 mm×2.1 mm,1.8 mm),以0.1%磷酸水-乙腈为流动相梯度洗脱,体积流量0.2 mL·min−1,进样量0.8 mL,柱温30℃;采用切换波长法测定15批PFSL中新绿原酸、绿原酸、咖啡酸、隐绿原酸、异槲皮苷、紫云英苷及异绿原酸C的含量,结合聚类分析(HCA)、主成分分析(PCA)和正交偏最小二乘法-判别分析(OPLS-DA)对含量测定结果进行综合评价。结果 新绿原酸、绿原酸、咖啡酸、隐绿原酸、异槲皮苷、紫云英苷及异绿原酸C在0.030 40~1.216 00、0.012 60~1.008 00、0.001 24~0.024 80、0.015 20~0.496 00、0.011 20~0.179 20、0.007 84~0.117 60、0.003 64~0.136 00 mg·mL−1线性关系良好(R2>0.999 0),平均加样回收率分别为96.01%、98.93%、98.52%、98.94%、98.06%、96.22%、98.20%,RSD分别为2.29%、3.13%、3.22%、2.71%、1.92%、2.86%、2.38%;质量分数分别为1.413 1~12.257 1、0.912 1~10.090 6、0.042 4~0.314 8、0.926 6~8.537 9、0.350 6~3.337 0、0.176 4~0.610 0、0.253 1~1.257 6 mg·g−1。化学计量学分析结果显示,15批PFSL样品聚为3类,隐绿原酸、咖啡酸、紫云英苷、新绿原酸、绿原酸、异槲皮苷为15批样品中的主要差异成分。结论 建立的UPLC含量测定方法稳定,结合化学计量学方法可为PFSL质量评价提供参考。
[Key word]
[Abstract]
Objective To establish an UPLC content determination method of seven components in Periploca forrestii stem-leaf (PFSL), and analyze the content determination results by chemometrics method. Methods The analysis was carried out on Agilent Eclipse Plus C18 column (100 mm×2.1 mm, 1.8 mm). The mobile phase was 0.1% phosphoric acid- acetonitrile with gradient elution. The volume flow was 0.2 mL·min−1, the injection volume was 0.8 μL, and the column temperature was 30℃. Measuring the content of neochlorogenic acid, chlorogenic acid, caffeic acid, cryptochlorogenic acid, isoquercitrin, astragalin and isochlorogenic acid C in 15 batches of PFSL by wavelength switching method. The content determination results were comprehensively analyzed using hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA).ResultsNeochlorogenic acid, chlorogenic acid, caffeic acid, cryptochlorogenic acid, isoquercitrin, astragalin and isochlorogenic acid C showed good linear relationship (R2>0.999 0) within the ranges of 0.030 40—1.216 00, 0.012 60—1.008 00, 0.001 24—0.024 80, 0.015 20—0.496 00, 0.011 20—0.179 20, 0.007 84—0.117 60, 0.003 64—0.136 00 mg·mL−1, whose average recoveries were 96.01%, 98.93%, 98.52%, 98.94%, 98.06%, 96.22% and 98.20%, with RSD values of 2.29%, 3.13%, 3.22%, 2.71%, 1.92%, 2.86%, 2.38%, respectively. Their mass fractions were 1.413 1—12.257 1, 0.912 1—10.090 6, 0.042 4—0.314 8, 0.926 6—8.537 9, 0.350 6—3.337 0, 0.176 4—0.610 0 and 0.253 1—1.257 6 mg·g−1. The chemometrics analysis results showed that 15 batches of PFSL could be clustered into three categories, cryptochlorogenic acid, caffeic acid, astragalin, neochlorogenic acid, chlorogenic acid and isoquercitrin were the main differential components in 15 batches of samples. Conclusion The established method for the determination of multi-component content in PFSL is stable, which can provide reference for the quality evaluation of PFSL combined with chemometrics method.
[中图分类号]
R284.1
[基金项目]
贵州省科技计划项目[黔科合基础-ZK(2022)一般475号];贵州省教育厅滚动支持省属高校科研平台团队项目[黔教技(2022)024号]