目的 建立HPLC-MS/MS同时测定同济2号颗粒中5个主要活性成分黄芪甲苷、绿原酸、人参皂苷Rg₁、人参皂苷Rb₁及三七皂苷R₁的方法。方法 以水(0.1%甲酸)-乙腈(0.1%甲酸)为流动相,梯度洗脱,体积流量为0.4 mL/min。YMC-Pack Pro C₈色谱柱分离,采用电喷雾离子源(ESI源),负离子模式,以选择性离子监测模式(SIM)进行测定。监测离子分别是m/z 829(黄芪甲苷)、m/z 353(绿原酸)、m/z 845(人参皂苷Rg₁)、m/z 1 108(人参皂苷Rb₁)、m/z 932(三七皂苷R₁)。结果 黄芪甲苷、绿原酸、人参皂苷Rg₁、人参皂苷Rb₁和三七皂苷R₁分别在0.075～2.4、0.95～30.3、1.71～54.72、1.12～35.92、0.45～14.28 μg/mL与峰面积呈良好线性关系。结论 该方法专属性好,灵敏度高,准确快捷,适用于同济2号颗粒的快速检测,为该药的质量标准提供依据。

Objective To establish an LC-MS/MS method for simultaneous determination of five compounds (astragaloside IV, chlorogenic acid, ginsenosides Rg₁, Rb₁, and notoginsenoside R₁) in Tongji No. 2 granules. Methods The chromatographic separation was carried out on a YMC-Pack Pro C₈ column (150 mm × 4.6 mm, 5 μm) eluted in a gradient program. The mobile phase consisted of water containing 0.1% formic acid-acetonitrile containing 0.1% formic acid. The mass spectra were obtained by Agilent QQQ triple quad mass spectrometer with electrospray ionization source in negative ion mode. Monitoring ions are m/z 829 (astragaloside IV), m/z 353 (chlorogenic acid), m/z 845 (ginsenosides Rg₁), m/z 1 108 (ginsenosides Rb₁), and m/z 932 (notoginsenoside R₁). Results The linear ranges for astragaloside IV, chlorogenic acid, ginsenosides Rg₁, ginsenosides Rb₁, and notoginsenoside R₁ were 0.075 - 2.4, 0.95 - 30.3, 1.71 - 54.72, 1.12 - 35.92, and 0.45 - 14.28 μg/mL. Conclusion The established method is convenient, sensitive, and accurate. It can be used for the determination of the contents of the main active ingredients in Tongji No. 2 granules for quality control.

上海市中西医结合重点病种建设项目(zxbz2012-15)