HPLC-Q-TOF-MS/MS法分析防己茯苓汤的化学成分

Chemical constituents of Fangji Fuling decoction by HPLC-Q-TOF-MS/MS

目的运用高效液相色谱-四极杆-飞行时间串联质谱法(HPLC-Q-TOF-MS/MS)对防己茯苓汤的化学成分进行快速分析与鉴定。方法采用Agilent Zorbax SB-C_(18)(4.6 mm×250 mm,5μm)色谱柱,以0.1%甲酸水-甲醇为流动相,梯度洗脱,进样量5μL,流速1.0 mL·min^(-1),柱后分流检测,分流比10∶1,柱温30℃。采用电喷雾离子源,在正负两种模式下进行质谱检测与分析。结果通过分析目标化合物的分子离子峰和二级质谱特征碎片离子,并且结合对照品裂解规律以及相关文献资料,共鉴定了其中36个化合物,包括7个生物碱类,13个萜类化合物,11个黄酮类化合物等。结论运用HPLC-Q-TOF-MS/MS技术可快速分析鉴定复方防己茯苓汤的主要化合物类型,对复方的质量控制及药效物质基础的进一步研究具有重要意义。

Objective To rapidly analyze and identify the main chemical constituents of Fangji Fuling decoction by ultra performance liquid chromatography quadrupole time of flight mass spectrometry(HPLC-Q-TOF-MS/MS).Methods The analysis was performed on Agilent Zorbax SB-C18(4.6 mm×250 mm,5μm),with 0.1%formic acid and methanol as the mobile phase in gradient elution.The column temperature was 30℃,the flow rate was 1.0 mL·min^(-1),the injection volume was 5μL,and the detection wavelength was 254 nm.The positive and negative electrospray ionization sources were used to determine the chromatographic effluent.Results Totally 36 compounds were identified,including 7 alkaloids,13 terpenoids and 11 flavonoids etc.,by analyzing the molecular ion peaks of the target compound and the characteristic fragment ions of MS/MS,and combining the reference substance fragmentation law and related literature.Conclusion The main chemical components of compound Fangji Fuling decoction can be rapidly analyzed and identified by HPLC-Q-TOF-MS/MS,which is of great significance to the further research of quality control and the material basis of the medicinal effect.