LC-MS法测定消癌平注射液中两种主要成分的含量

Simultaneous Determination of Two Major Compound in Xiao Aiping Injection by LC-MS

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： A rapid and specific high performance liquid chromatography-mass spectrometric method was developed for determination of 17β-tenacigenin B and tcnacigenoside A in Xiaoaiping injection. Method： The analytical column was Agilent Zorhax SB-C18 （3.0 mm× 100 mm, 3.5 μm） and the security guard column was Agilent Zorhax SB-C18 （2. 1 mm× 12.5 mm, 5 μm）. The mobile phase was methanol-water （90： 10） at a flow rate of 0, 25 mL ·min^-1. Methyhestosterone was used as internal standard; electrospray ionization model （ES1） and SIM model were used for quantification. Result： The linear ranges of two compounds were as follows ： 0. 625-20 mg ·L^-1 （r =0. 998 3） for 17β-tenacigenin B, 0. 375-12 mg ·L^-1 （r =0. 999 4） for tenacigenoside A. The average recoveries Were 100.8% （RSD 3.95% ） , 101.6% （RSD 2.71% ） , respectively. Conclusion： This established method was sensitive, fast, accurate and available for the quality control of Xiaoaiping Injection.