超快速液相色谱-三重四级杆/线性离子阱质谱法比较分析竹节参根与根茎中多元指标成分

Comparative Analysis of Multiple-Index Constituents in Roots and Rhizomes of Panax japonicus by UFLC-QTRAP-MS/MS

    摘要
  • 摘要:
      目的  建立超快速液相色谱-三重四级杆/线性离子阱质谱法(UFLC-QTRAP-MS/MS)同时测定竹节参根与根茎中皂苷、氨基酸及核苷类共33种成分含量的方法。
      方法  采用XBridge®C18(4.6 mm×100 mm, 3.5 μm), 以0.1%甲酸水-0.1%甲酸乙腈为流动相, 梯度洗脱, 流速0.8 mL·min-1, 柱温30 ℃, 多反应监测离子扫描模式(MRM)测定。根据33种目标成分的含量, 采用聚类、非线性映射及主成分分析进行综合评价。
      结果  33种成分在一定浓度范围内均呈现良好的线性关系, 相关系数均大于0.999 0;精密度、重复性和稳定性良好; 平均加样回收率为96.90%~101.6%, RSD均≤3.6%。统计分析结果显示从33种成分的含量角度, 竹节参根与根茎中皂苷、氨基酸及核苷类成分较为相似。
      结论  所建立的方法准确、可靠, 可为竹节参药材内在质量的综合评价和全面控制提供新的方法参考, 同时为竹节参根的开发利用提供基础资料。

     

    Abstract:
      OBJECTIVE  To develop a method for the determination of saponins, amino acids and nucleosides in roots and rhizomes of Panax japonicus by UFLC-QTRAP-MS/MS.
      METHODS  The extract was separated on a XBridge®C18(4.6 mm×100 mm, 3.5 μm) at 30 ℃ with a gradient elution of 0.1% formic acid solution -0.1% formic acid acetonitrile, and the flow rate was 0.8 mL·min-1, using multiple-reaction monitoring (MRM) mode. Hierarchical cluster, nonlinear mapping and principal component analysis were adopted for comparison of roots and rhizomes.
      RESULTS  33 constituents showed good linearity (r>0.999 0) in the range of the tested concentration; the precision, repeatability and stability were good; the average recovery rates were between 96.90% and 101.6%, the relative standard deviations were less than or equal to 3.6%.
      CONCLUSION  The results of data analysis showed that roots were similar to rhizomes according to contents of 33 constituents. The established method was accurate and reliable, which could used as a reference for quality evaluation and comprehensive control of Panax japonicus, and provided basic information for the development and utilization of roots of Panax japonicus.

     

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