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

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 C_(18)(4.6 mm×100 mm,3.5μm),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0.9990;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。

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 C_(18)(4.6 mm×100 mm,3.5μm)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>0.9990)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.