UHPLC-ESI-MS/MS测定复方景川片中6种成分的含量

Simultaneous Determination of 6 Components in Compound Jingchuan Tablets by UHPLC-ESI-MS/MS

关键词:  液质联用  复方景川片  没食子酸  红景天苷  绿原酸  多重反应监测

Key words:  UHPLC-ESI-MS/MS  Compound Jingchuan tablets  gallic acid  salidroside  chlorogenic acid  MRM

摘要:

目的 采用UHPLC-ESI-MS/MS同时测定复方景川片中没食子酸、红景天苷、绿原酸、延胡索乙素、阿魏酸、欧当归内酯A的含量。方法 采用InertSustain^® C₁₈（3.0 mm×100 mm，3.0 μm）色谱柱，乙腈-0.1%甲酸水溶液，梯度洗脱，流速0.4 mL·min^-1，进样量10 μL；质谱采用电喷雾离子源（ESI源），正负离子扫描切换，多重反应监测模式进行定量分析。结果 复方景川片中6种成分的峰面积与质量浓度在一定范围内均呈良好的线性关系，仪器精密度RSD值<2.5%，加样回收率为98.56%~102.04%，RSD为0.97%~2.07%。在所设定的色谱条件下，复方景川片中6个成分（没食子酸、红景天苷、绿原酸、延胡索乙素、阿魏酸、欧当归内酯A）于11 min内完全分离。结论 建立的UHPLC-ESI-MS/MS方法快速简便、精密度好、灵敏度高，可用于复方景川片的质量控制。

Abstract:

OBJECTIVE To develop a method for simultaneous determination of gallic acid, salidroside, chlorogenic acid, tetrahydropalmatine, ferulic acid and levistolide A in Compound Jingchuan tablets by UHPLC-ESI-MS/MS. METHODS The separation was performed on a InertSustain^® C₁₈ (3.0 mm×100 mm, 3.0 μm) column, mobile phase consisting of water (containing 0.1% formic acid) and acetonitrile with gradient elution at a flow rate of 0.4 mL·min^-1, and the injection volume was 10 μL. Multiple-reaction monitoring (MRM) was employed with switching electrospray ion source polarity in positive and negative mode. RESULTS There was a good linear relationship between the peak area and the mass concentration of the 6 components in Compound Jingchuan tablets. The RSD of precision were <2.5%, the average recoveries ranged of 98.56%-102.04%, RSD ranged of 0.97%-2.07%. Under the optimized chromatographic conditions, the complete separation of 6 target components were obtained within 11 min. CONCLUSION The established UHPLC-ESI-MS/MS can be served as a scientific and effective way for quality control of Compound Jingchuan tablets.