LC-MS/MS同时测定刺五加中刺五加苷E、异嗪皮啶、绿原酸、原儿茶酸和齐墩果酸的含量

Simultaneous Determination of Eleutheroside E, Isothiazine, Chlorogenic Acid, Protocatechuic Acid and Oleanolic Acid in Acanthopanax by LC-MS/MS

摘要: 目的：建立一次测定刺五加中刺五加苷E、异嗪皮啶、绿原酸、原儿茶酸和齐墩果酸的含量的方法。方法 采用超高效液相色谱－质谱联用(UPLC-MS/MS)法。质谱条件：采用电喷雾离子源，正离子扫描模式，多离子反应监测扫描方式；采用外标法进行定量分析。结果：刺五加苷E、异嗪皮啶、绿原酸、原儿茶酸和齐墩果酸五种物质的含量分别在10~10,000 mg/mL、0.1~5000 mg/mL、1~10,000 mg/mL、 0.1~ 10,000 mg/mL 和100~30,000 mg/mL浓度范围内，线性关系良好，R2均 > 0.9993；加标实验回收率在94.67%~98.03%之间。结论 此方法灵敏度高、选择性好、分析时间短，可以对刺五加中刺五加苷E、绿原酸、齐墩果酸、异嗪皮啶和原儿茶酸进行准确的定量分析。

Abstract: Objective: To establish an UPLC-MS/MS method for the simultaneous determination of eleutheroside E, sofraxidin, chlorogenic acid, protocatechuate and oleanolic acid in Acanthopanax Stems and leaves. Methods: water-methanol is used as mobile phase to operate gradient elution; Flowing Speed: 0.25 mL/min; Temperature: 25˚C; Injection volume: 10 μL. Mass Condition: ESI ion source, positive, MRM scanning mode is used, and external standard method is used to ration. Results: eleutheroside E, sofraxidin, chlorogenic acid, protocatechuate and oleanolic acid have good linear relationship by the range of 10 - 10,000 mg/mL, 0.1 - 5000 mg/mL, 1 - 10,000 mg/mL, 0.1 - 10,000 mg/mL and 100 - 30,000 mg/mL respectively, and R2 > 0.9993 in all over. The spiked recovery is between 94.67% - 98.03%. This method is successfully applied to measure the contents of target compound in wild and cropped Acanthopanax senticosus (Rupr. Maxim.) Harms stem and leaf. Conclusions: This method has the advantages of high sensitivity, good selectivity and shorter analysis time, and can be applied to make accuracy quantitative analysis for the eleutheroside E, sofraxidin, chlorogenic acid, protocatechuate and oleanolic acid in Acanthopanax.