广西桑寄生中多元活性成分动态积累的分析与评价

Analysis and evaluation of dynamic accumulation of multiple active constituents in Taxilli Herba in Guangxi

建立超高效液相色谱-三重四极杆/线性离子阱质谱(UHPLC-QTRAP-MS/MS)同时测定桑寄生中黄酮、有机酸、核苷和氨基酸共33种活性成分含量的方法,并对其多元活性成分的动态积累进行分析与评价。采用XBridge C_(18)色谱柱(4.6 mm×100 mm,3.5μm),以0.1%甲酸水-甲醇为流动相进行梯度洗脱,流速0.5 mL·min^(-1),柱温30℃,进样量为2μL;质谱采用电喷雾离子源(ESI),多反应离子监测(MRM)模式测定;采用熵权TOPSIS法对各项指标成分客观赋权,根据相对贴近度(C_(i))进行综合排序,构建桑寄生多指标综合评价模型。结果表明,33种目标成分的浓度和峰面积在各自线性范围内具有良好的线性关系,相关系数(r)均不小于0.9990;精密度、重复性、稳定性RSD≤4.7%;平均加样回收率为98.03%~101.3%,RSD均小于4.0%。桑寄生中各成分的积累动态不一,2月中旬至3月初采收的桑寄生药材综合质量较好,与当地传统采收期相符。该研究为揭示桑寄生中多元活性成分的动态积累规律及确定其药材的适宜采收期提供基础资料,同时为桑寄生药材内在质量的综合评价提供新的方法参考。

A method based on ultra-high performance liquid chromatography with triple quadrupole/linear ion trap mass spectrometry(UHPLC-QTRAP-MS/MS)was developed for the simultaneous determination of 33 active constituents,including flavonoids,organic acids,nucleosides,and amino acids in Taxilli Herba to analyze and evaluate the dynamic accumulation of their multiple active constituents.The separation was performed at 30℃on an XBridgeC_(18) column(4.6 mm×100 mm,3.5μm)with gradient elution using 0.1%formic acid aqueous solution-methanol as the mobile phase at a flow rate of 0.5 mL·min^(-1),and the injection volume was 2μL.The constituents were ionized in the electrospray ionization source(ESI)and quantitated by the multiple reaction monitoring(MRM)mode.The entropy weight TOPSIS method was used to objectively assign weights to the target constituents and rank them according to their relative closeness coefficient(C_(i))to construct a multi-index comprehensive evaluation model of Taxilli Herba.The results showed that the concentrations and peak areas of 33 target constituents had good linearity in their respective linear ranges,and the correlation coefficients(r)were not less than 0.9990.The RSD of precision,reproducibility,and stability were not higher than 4.7%.The average recoveries were 98.03%-101.3%with RSD less than 4.0%.There were differences in the content of 33 active constituents in Taxilli Herba at different harvest periods.The overall quality of Taxilli Herba harvested from mid-February to early March was better,which was consistent with the traditional harvest period.This study provides basic information for revealing the rule of dynamic accumulation of multiple active constituents in Taxilli Herba and determining the suitable harvesting period.Meanwhile,it also provides a new methodological reference for the comprehensive evaluation of the intrinsic quality of Taxilli Herba.