HPLC-QTOF-MS分析六味地黄丸不同部位的化学成分

Analysis of Chemical Constituents of Different Polarity Fractions from Liuwei Dihuang Pills by HPLC-QTOF-MS

目的采用高效液相色谱—四级杆—飞行时间串联质谱(HPLC-QTOF-MS)法对六味地黄丸不同极性溶剂提取部位中的化学成分进行鉴定,并比较不同极性提取部位之间的成分差异。方法色谱分离采用WatersXBridge BEH C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)和0.1%甲酸溶液(B)为流动相梯度洗脱,流速为0.6 m L·min^(-1);质谱采用电喷雾离子源(ESI),在正负离子模式下扫描采集数据,根据准分子离子及二级碎片离子,并结合对照品及文献报道的质谱数据对六味地黄丸不同极性溶剂提取部位中的化学成分进行鉴定。结果从六味地黄丸的水、50%乙醇、75%乙醇、乙醇、石油醚和混合溶剂提取部位中分别鉴定出41、41、41、40、7和39个化合物。结论本研究首次对六味地黄丸的不同极性提取部位中的化学成分进行了鉴定和对比分析,丰富了六味地黄丸化学成分的结构信息,可为六味地黄丸的药效物质研究提供了科学参考。

Objective To identify the chemical constituents and compare differences of six different polarityextracted fractions from Liuwei Dihuang pills by a high-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry（HPLC-QTOF-MS）. Methods The analysis was performed on Waters XBridge BEH C_（18）（4.6 mm × 250 mm,5 μm） with gradient elution of acetonitrile（A） and 0.1% formic acid（B） at the flow rate of0.6 m L·min^（-1）. Mass spectrometric data were obtained under electrospray ionization（ESI） in negative and positivemodes. The compounds from Liuwei Dihuang pills were confirmed according to MS spectra and MS/MS fragments,comparing experimental spectroscopic data to standard values,and consulting the relevant literatures. Results 41,41,41,40,7 and 39 constituents were identified from water,50% ethanol,75% ethanol,ethanol,petroleumether and mixed solvents extracted fractions, respectively. The compounds identified were finally marked on thecorresponding chromatograms. Conclusion The chemical compounds in different polarity extracted fractions of Liuwei Dihuang pills were firstly analyzed in this study,which provided a foundation for the research of effectivesubstance of Liuwei Dihuang pills.