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

关键词:  消癌平注射液  通关藤苷A  通关藤苷I  通关藤苷H  超高效液相色谱-串联质谱法  含量测定

Key words:  Xiaoaiping injection  Tenacissoside A  Tenacissoside H  Tenacissoside I  UPLC-MS/MS  content determination

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.