HPLC-ESI/MS测定消癌平注射液中3种主要成分的含量

Simultaneous determination of 3 major compounds in Xiaoaiping injection by HPLC-ESI/MS

目的建立同时测定消癌平注射剂中3种主要成分通关藤皂苷H、G、I质量分数的液相色谱-质谱联用法。方法色谱柱为Agilent Zobax SB-C18色谱柱（4.6 mm×150 mm,5.0μm）,流动相为乙腈-0.1%（体积分数）甲酸（体积比53∶47）,流速为1.0 m L/min,内标物为利福布汀,质谱采用电喷雾电离化（ESI）方式,正离子检测,以选择离子反应监测（SIR）模式对3种甾体皂苷进行质量分数测定。结果通关藤皂苷H、G、I的线性范围分别为0.109 5~4.38μg/m L（r=0.999 0）、0.12~4.00μg/m L（r=0.9994）、0.127~5.08μg/m L（r=0.999 6）,加样回收率分别为100.8%（RSD=3.17%）、100.3%（RSD=2.01%）和98.9%（RSD=2.27%）。结论本方法精密度高、快速简便,可为消癌平注射液的质量控制提供依据。

Objective A rapid and specific HPLC-ESI / MS method was developed for determinantion of tenacissoside H,G and I in Xiaoaiping injection. Methods The analytical column was Agilent Zobax SBC18（ 4. 6 mm × 150 mm,5. 0 μm）. The mobile phase was acetonitrile and 0. 1% HCOOH（ 53∶ 47） at a flow rate of 1. 0 m L / min. Rifabutin was used as internal standard. Electrospray ionization model（ ESI）and SIR model were used for quantification. Results The linear ranges were as follows： 0. 109 5- 4. 38μg /m L（ r = 0. 999 0） for tenacissoside H,0. 12- 4. 00 μg /m L（ r = 0. 999 4） for tenacissoside G,and 0.127- 5. 08 μg / m L（ r = 0. 999 6） for tenacissoside I. The average recoveries were 100. 8%（ RSD = 3.17%）,100. 3%（ RSD = 2. 01%） and 98. 9%（ RSD = 2. 27%）,respectively. Conclusion This method is sensitive,fast and simple,which could be used for the quality control of Xiaoaiping injection.