基于UPLC-LTQ-Orbitrap-MS方法分析半夏泻心汤化学成分

Identification of chemical constituents in Banxia Xiexin decoction based on UPLC-LTQ-Orbitrap-MS

目的:基于超高效液相色谱-离子阱-静电场轨道阱质谱(UPLC-LTQ-Orbitrap-MS)技术鉴定半夏泻心汤化学成分。方法:采用Dikma Endeavorsil C18色谱柱(100 mm×2.1 mm,1.8μm),以0.1%甲酸水-乙腈为流动相体系,梯度洗脱,流速0.3 mL·min-1,质谱采用电喷雾(ESI)离子源,以正、负离子模式采集多级质谱碎片信息。结果:通过对照品比对、精确相对分子质量、多级质谱碎片信息,结合文献报道,从半夏泻心汤中鉴定出99个化学成分,包括54个黄酮类、10个生物碱类和16个皂苷类化合物,还有脂肪酸类、酚酸类、醇类、内酯等其他成分。结论:本研究建立的分析方法灵敏、高效,可应用于半夏泻心汤各类化学成分的鉴定分析,为研究半夏泻心汤药效物质基础和作用机制提供重要依据。

Objective:To identify the chemical constituents of Banxia Xiexin decoction by using the ultra performance liquid chromatography coupled with linear quadrupole ion trap-orbitrap mass spectrometry(UPLCLTQ-Orbitrap-MS). Methods:The separation was performed on a Dikma Endeavorsil C18 column(100 mm×2.1 mm,1.8 μm) with mobile phase of water(containing 0.1% formic acid)-acetonitrile with gradient elution at a flow rate of 0.3 mL·min-1. LTQ-Orbitrap-MS with electrospray ion(ESI) source was applied to collect multi-level mass spectrometry fragment information under positive and negative ion modes. Results:A total of 99 chemical components were identified by reference substance comparison,accurate molecular weight,multilevel mass spectrometry fragments and related literature reports,including 54 flavonoids,10 alkaloids and 16 saponins,as well as fatty acids,phenolic acids,alcohols and lactones components. Conclusion:The proposed method is sensitive and efficient,and can be applied in identification analysis of various chemical constituents of Banxia Xiexin decoction,which provides a crucial basis for further studying the material of its efficacy and mechanism.