基于GC-TOF-MS和UHPLC-QE-MS的苏合香化学成分分析

Chemical constituents in the extract of styrax by GC-TOF-MS and UHPLC-QE-MS

目的 基于GC-TOF-MS和UHPLC-QE-MS分析中药苏合香的化学成分。方法 挥发性成分分析采用Agilent DB-5MS毛细管色谱柱(30 m×250μm×0.25μm);程序升温,进样口温度280℃;柱流速1.0 mL·min^(-1);进样量1μL;分流比15:1;通过标准谱库检索并结合文献对主要色谱峰进行鉴定。可溶性成分分析采用Waters ACQUITY UPLC HSS T3色谱柱(2.1mm×100 mm,1.8μm);流动相为5.0 mmol·L^(-1)乙酸铵-5.0 mmol·L^(-1)乙酸和乙腈;梯度洗脱;NCE模式下碰撞能量;电喷雾离子源正负离子模式下对色谱流出物进行质谱检测,利用对照品、二级质谱信息及文献对各主要色谱峰进行归属。结果 苏合香提取物中共鉴定出25个挥发性成分和32个可溶性成分。结论 该方法准确稳定,重复性好,可用于苏合香的成分分析。

Objective To determine the chemical components in traditional Chinese medicine styrax with GC-TOF-MS and UHPLC-QE-MS.Methods Agilent DB-5MS capillary chromatography column(30 m×250 μm×0.25 μm) was used for the volatile components.Programmed temperature rise was used,with the sample inlet temperature at 280 ℃.The flow rate was 1.0 mL·min^(-1),the injection volume was 1 μL,and the split ratio was 15∶1.The standard spectrum library was retrieved and the main chromatographic peaks were identified based on literatures.Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm) was used for the soluble components.The mobile phase consisted of 5.0 mmol·L^(-1) ammonium acetate-5.0 mmol·L^(-1) acetic acid and acetonitrile,with gradient elution.Collision energy was used in NCE mode.The chromatographic effluents were detected by mass spectrometry in both positive and negative ion mode of the electrospray ion source.The main chromatographic peaks were assigned with the reference substance,secondary mass spectrometry information and related literatures.Results Totally 25 volatile components and 32 soluble components were identified in the extract of styrax.Conclusion This method is accurate,stable,and repeatable,and can be used for the determination of components in styrax.