不同加工竹节参中多元活性成分同时测定及灰色关联度分析

Stimultaneous determination of multiple bioactive constituents in Panacis Japonici Rhizoma processed by different methods and grey relational analysis

建立超快速液相色谱-三重四极杆/线性离子阱质谱(UFLC-QTRAP-MS/MS)同时测定竹节参中皂苷、氨基酸及核苷类共33种成分含量的方法,考察不同加工方法对竹节参药材中目标成分的影响。采用XBridge■C18(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;用灰色关联度分析(GRA)对不同加工竹节参进行综合分析与评价。结果表明,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95.33%~101.8%,RSD均小于5%。GRA评价结果显示,微波干燥、完整根茎不去皮的竹节参样品综合质量较好。所建立的方法准确、可靠,可用于竹节参药材内在质量的综合评价,该研究可为竹节参适宜产地加工方法的优选及其加工方法的规范化和标准化提供基础资料。

A method, for determination of saponins, amino acids and nucleosides in Panacis Japonici Rhizoma of ultra fast liquid chromatography with triple quadrupole linear ion trap mass spectrometry(UFLC-QTRAP-MS/MS), was established to investigate the effect of different processing methods on the target components of Panacis Japonici Rhizoma. The chromatographic separation was performed 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. The grey relational analysis was adopted for the analysis of different processing samples. The results showed that the thirty-three constituents were in a good linear range and the correlation coefficient was greater than 0.999 0;the precision, repeatability and stability were good;the average recovery rates were between 95.33% and 101.8%, and the relative standard deviations were less than 5%. The result of grey relational analysis showed that the complete rhizomes without peeling, which were adopted for the microwave dried method, had the best quality. The established method was accurate and reliable, which could be used to appraise the quality of Panacis Japonici Rhizoma. Our study may lay the way for the processing method of Panacis Japonici Rhizoma in optimization,normalization and standardization.