基于HPLC-QAMS及特征图谱的小木通藤茎质量评价

Quality Evaluation of the Rattan Stems of Clematis armandii Based on HPLC-QAMS and Characteristic Chromatogram

目的:基于HPLC-QAMS及特征图谱对小木通藤茎的质量进行评价。方法:使用WondaCract ODS-2(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.3%甲酸溶液为流动相,梯度洗脱;柱温为30℃;流速为1.0 mL/min;检测波长为316 nm;进样量为10μL,建立小木通藤茎HPLC特征图谱,对数据进行聚类分析、主成分分析和正交偏最小二乘判别分析。以阿魏酸为内标,计算香草醛、咖啡酸的相对校正因子,并利用一测多评法测定其含量。结果:建立的小木通藤茎HPLC特征图谱标定12个共有峰,并指认其中3个成分,15批小木通藤茎的HPLC特征图谱与对照图谱的相似度≥0.938。化学计量学分析结果显示小木通藤茎的分类呈现出一定的区域相关性。15批小木通藤茎样品中咖啡酸、香草醛和阿魏酸的含量分别为0.0212~0.1018 mg/g、0.0141~0.0360 mg/g、0.0234~0.0659 mg/g。QAMS与外标法测得结果无显著差异。结论:所建立的小木通藤茎HPLC特征图谱和含量测定方法简便可行、快速准确,可为小木通藤茎的质量控制提供参考。

Objective:To evaluate the quality of the rattan stems of Clematis armandii based on HPLC-QAMS and characteristic chromatogram.Methods:The Chromatographic separation was performed on the WondaCract ODS-2(250 mm×4.6 mm,5μm)column,the mobile phase was acetonitrile-0.3%formic acid with gradient elution.The flow rate was 1.0 mL/min,column temperature was 30℃,detection wavelength was 316 nm,injection volume was 10μL.The HPLC characteristic chromatogram of the rattan stems of Clematis armandii was established,and cluster analysis,principal component analysis,orthogonal partial least squares discriminant analysis were carried on.With ferulic acid as internal standard,the relative correction factors of vanillin and caffeic acid were calculated and their contents were determined by one test and multiple evaluation method.Results:The HPLC characteristic chromatogram of the rattan stems of Clematis armandii was established.Twelve characteristic peaks were determined and three components were identified.The similarity between HPLC chromatograms and control chromatograms of rattan stems of 15 batches of Clematis armandii was equal or greater than 0.938.The results of chemometric analysis showed that the classification of the rattan stems of Clematis armandii revealed regional correlation.The contents of caffeic acid,vanillin and ferulic acid in 15 batch samples of the rattan stems of Clematis armandii were 0.0212 to 0.1018 mg/g,0.0141 to 0.0360 mg/g,0.0234 to 0.0659 mg/g.There was no significant difference between QAMS and ESM.Conclusion:The established HPLC chromatogram and content determination method were simple,feasible,rapid and accurate,and can provide reference for the quality control of the rattan stems of Clematis armandii.