杏苏散的全成分飞行时间质谱分析及主要化学成分鉴定

Identification of Major Components of Xingsusan Decoction by HPLC-HR-TOF /MS

目的:采用高效液相-高分辨飞行时间质谱(HPLC-HR-TOF/MS)技术,对杏苏散水煎液中的化学成分进行初步分析。方法:采用Welchrom-C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-水(含体积比0.1%甲酸)为流动相,梯度洗脱,流速为1.0 mL/min,ESI-TOF-MS正负离子Auto MSn采集模式。通过HPLC-TOF-MS得到化合物分子量以及MS/MS CID碰撞解离碎片,结合文献报道,对杏苏散水煎液的主要化学成分进行分析鉴定。结果:结合文献报道和飞行时间质谱数据,通过色谱柱分离检测到上百个成分,通过分子量以及MS/MS裂解碎片对其中52个化合物进行了初步鉴定。结论:HPLC-HR-TOF/MS技术是鉴定复杂中药复方成分的有效手段,对阐明复方作用的物质基础、探讨其作用机制及其质量控制有重要意义。

Objective：The major components of Xingsusan decoction were studied by HPLC-HR-TOF-MS. Methods：A WelchromC18column（4. 6 mm × 250 mm,5 μm）was used at a flow rate of 1. 0 mL /min. The HPLC gradient was acetonitrile-formic acid（99. 9 ∶0. 1,V /V）（B）and water-formic acid（99. 9 ∶ 0. 1,V /V）（ A）. HR-MS /MS analysis were carried out using a Micro /TOF-Q Ⅱ Focus mass spectrometer fitted with an ESI source operating in Auto-MSnmode to obtain fragment ions. TIC chemical profiles of the extract were established in both positive and negative modes. The structures of the known components in Xingsusan decoction were identified by comparing their retention times,molecular weight and CID fragmentation patterns with their corresponding compounds reported in the literature. Results：A total of 52 components were simultaneously detected in Q-TOF /MS. Conclusion：This method can be used as reference for other Chinese Medicine formulas study.