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目的:建立同时测定消癌平注射液中两种甾体皂苷17β-tenacigenin B和tenacigenoside A含量的液相色谱-质谱联用法。方法:Agilent Zorbax SB-C18色谱柱(3.0×100 mm,3.5μm),保护柱为Agilent Zorbax SB-C18(2.1×12.5 mm,5μm),流动相甲醇-水(90∶10),流速0.25 mL·min-1。甲睾酮为内标,质谱采用电喷雾离子化(ESI)方式,正离子采集,以选择离子反应监测(SIR)模式对两种甾体皂苷进行含量测定。结果:17β-tenacigenin B和tenacigenoside A的线性范围分别为0.625～20mg·L-1(r=0.998 3),0.375～12 mg·L-1(r=0.999 4),加样回收率分别为100.8%(RSD 3.95%)101.6%,(RSD 2.71%)。结论:该方法简便,准确,重复性好,可为消癌平注射液提供质量控制依据。
OBJECTIVE: To establish a liquid chromatography-mass spectrometry (LC-MS) method for the simultaneous determination of 17β-tenacigenin B and tenacigenoside A in Xiaojianping injection. Methods The Agilent Zorbax SB-C18 column (3.0 × 100 mm, 3.5 μm) was used. The guard column was Agilent Zorbax SB-C18 (2.1 × 12.5 mm, 5 μm) · Min-1. Methyltestosterone was used as internal standard. The mass spectrometry was carried out by electrospray ionization (ESI) and positive ion. The content of two steroidal saponins was determined by selective ion monitoring (SIR). Results: The linear range of 17β-tenacigenin B and tenacigenoside A were 0.625 ~ 20 mg · L -1 (r = 0.998 3) and 0.375 ~ 12 mg · L -1 (r = 0.999 4) respectively. The recovery rates were 100.8 % (RSD 3.95%) 101.6%, (RSD 2.71%). Conclusion: The method is simple, accurate, reproducible, and can provide quality control basis for Xiao-Jin-Ping injection.