不同加工麦冬中多元活性成分的含量测定及多元统计分析

Determination of multiple bioactive constituents in Ophiopogonis Radix processed by different methods and multivariate statistical analysis

目的: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)同时测定麦冬中甾体皂苷、高异黄酮、氨基酸及核苷类共32个成分含量的方法,考察不同加工方法对麦冬药材中多元活性成分的影响。方法:采用SynergiTM Hydro-RP 100?柱(2.0 mm×100 mm,2.5μm),以0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相,梯度洗脱,流速0.4 mL·min-1,柱温30℃,多反应离子监测(MRM)模式检测;用灰色关联度分析(GRA)和TOPSIS方法对多元活性成分进行综合评价。结果:32个成分在一定浓度范围内线性关系良好,相关系数均大于0.999 0;精密度、重复性、稳定性良好,RSD均小于5%;平均加样回收率为97.4%~102.0%,RSD均小于5%。GRA和TOPSIS分析结果显示,S5、S6样品综合质量较好。结论:所建立的方法准确、可靠,可用于麦冬药材内在质量的综合评价,该研究可为麦冬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。

Objective:To investigate the influence of different processing methods on components in Ophiopogonis Radix,and establish a comprehensive analytical method using UFLC-QTRAP-MS/MS for the simultaneous determination of thirty-two components including steroidal saponins,homoisoflavonoids,amino acids and nucleosides in Ophiopogonis Radix.Methods:The chromatographic separation was performed on a SynergiTM Hydro-RP 100?column(2.0 mm×100 mm,2.5μm)at 30℃with a gradient elution of 0.1%formic acid solution-0.1%aqueous formic acid at a flow rate of 0.4 mL·min-1.The components were detected under multiple-reaction monitoring(MRM)mode.Besides,grey relation analysis(GRA)and TOPSIS methods have been applied to comprehensively analyze and evaluate the results of multiple active constituents.Results:The results showed that thirty-two components had good linearity with correlation coefficients above 0.999 0.The method exhibited good precision,repeatability and stability with the relative standard deviations(RSDs)less than 5%,the average recoveries were between 97.4%and 102.0%with RSDs below 5%.In addition,the results of GRA and TOPSIS indicated that the quality of S5 and S6 was better.Conclusion:The established method is accurate and reliable,which can be used to appraise the quality of Ophiopogonis Radix.Our study may lay the way for the processing method of Ophiopogonis Radix in optimization,normalization and standardization.