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目的采用LC-MS法同时测定清热养心颗粒中的绿原酸、咖啡酸、甘草次酸、氧化苦参碱和薯蓣皂苷元。方法色谱柱为Agilent Zorbax SB C18柱(100 mm×3.0 mm,3.5μm),流动相为水-甲醇(10∶90),柱温40℃,流速0.2 m L·min-1,进样量10μL,离子化方式为电喷雾(ESI),选择性离子检测(SIR),正负离子同时检测,检测电压3.5 k V,离子源温度120℃,脱溶剂温度450℃,脱溶剂气体为N2,体积流量480 L·h-1。结果绿原酸、咖啡酸、甘草次酸、薯蓣皂苷元和氧化苦参碱的线性范围分别为11.60~2.97×103(r=0.9986)、3.05~780(r=0.9958)、1.10~282(r=0.9991)、3.63~930(r=0.9931),0.47~120μg·L-1(r=0.9977)。结论所用方法专属性强、快速灵敏、可用于清热养心颗粒中绿原酸、咖啡酸、甘草次酸、氧化苦参碱、薯蓣苷元等成分的含量测定。
Objective To determine the contents of chlorogenic acid, caffeic acid, glycyrrhetinic acid, oxymatrine and diosgenin in Qingre Yangxin Granules by LC-MS method. Methods The column was Agilent Zorbax SB C18 column (100 mm × 3.0 mm, 3.5 μm). The mobile phase was water-methanol (10:90) and the column temperature was 40 ℃. The flow rate was 0.2 mL · min-1. (ESI), selective ion detection (SIR), simultaneous detection of positive and negative ions, detection voltage 3.5 kV, ion source temperature 120 ℃, desolvation temperature 450 ℃, desolvation gas N2, volume flow rate 480 L · h-1. Results The linear ranges of chlorogenic acid, caffeic acid, glycyrrhetinic acid, diosgenin and oxymatrine were 11.60-2.97 × 103 (r = 0.9986), 3.05-780 (r = 0.9958), 1.10-282 = 0.9991), 3.63 ~ 930 (r = 0.9931), 0.47 ~ 120μg · L-1 (r = 0.9977). Conclusion The method used is specific, rapid and sensitive and can be used for the determination of chlorogenic acid, caffeic acid, glycyrrhetinic acid, oxymatrine and dysenteryin in Qingre Yangyangxin granules.