UPLC-MS/MS同时检测消癌平注射液中通关藤苷A、I、H的含量

    Simultaneous Determination of Tenacissoside A, Tenacissoside H and Tenacissoside I in Xiaoaiping Injection by UPLC-MS/MS

    • 摘要: 目的 建立UPLC-MS/MS同时测定消癌平注射液中通关藤苷A、通关藤苷I、通关藤苷H的含量。方法 采用Phenomenex Kinetex XB-C18色谱柱(2.1 mm×50 mm,2.6 μm),以0.1%甲酸水-乙腈为流动相,梯度洗脱分离,流速为0.2 mL·min-1,通过电喷雾离子源,多反应监测(MRM),正离子模式。结果 通关藤苷A、I、H分别在0.05~10 ng·mL-1,0.025~10 ng·mL-1,0.025~10 ng·mL-1浓度内呈良好的线性关系,r>0.998,检测限为0.012 5~0.025 ng·mL-1,平均回收率分别为97.9%,95.7%,96.1%,RSD<3.4%。结论 方法简单快速,准确灵敏,可用于消癌平注射液中通关藤苷A、I、H的定量测定。

       

      Abstract: OBJECTIVE to establish a method for the simultaneous determination of Tenacissoside A, Tenacissoside H and Tenacissoside I in Xiaoaiping injection by UPLC-MS/MS. METHODS The separation was performed on a Phenomenex Kinetex XB-C18 column(2.1 mm×50 mm, 2.6 μm) using the mobile phase of acetonitrile-0.1% formic acid solution at a flow rate of 0.2 mL·min-1 in gradient elution mode. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring via electrospray ionization source in positive mode. RESULTS The linearity range of Tenacissoside A, Tenacissoside H and Tenacissoside I were 0.05-10 ng·mL-1, 0.025-10 ng·mL-1, 0.025-10 ng·mL-1, respectively, with all correlation coefficient (r) >0.998. The limit detection was 0.012 5-0.025 ng·mL-1 and the recoveries were 97.9%, 95.7%, 96.1%, respectively, with RSD <3.4%. CONCLUSION The proposed UPLC-MS/MS method is simple, rapidness, accurate, and sensitivity, can be used for the quantitative determination of Tenacissoside A, Tenacissoside H and Tenacissoside I in Xiaoaiping injection.

       

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