UPLC-MS/MS法同时测定鼠曲草中的咖啡酸、原儿茶酸和绿原酸

Simultaneous determination of caffeic acid,protocatechuic acid and chlorogenic acid in Gnaphalium affine by UPLC-MS/MS

目的建立超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定鼠曲草中3种有机酸类成分(咖啡酸、原儿茶酸和绿原酸)的含量。方法采用负离子多反应监测模式进行含量测定。色谱条件:采用Kinnetex C18(2.1 mm×100 mm,2.6μm)色谱柱,以乙腈(A)-0.1%氨水(B)为流动相,梯度洗脱,流速0.25 ml/min,柱温40℃。结果3种有机酸类成分在考察的线性范围内呈良好的线性关系(r>0.9984),精密度、稳定性和重复性考察符合分析要求,回收率和RSD分别在95.00%~102.55%和2.42%~3.06%。6批样品中3个化学成分的含量测定结果为咖啡酸10.25~45.12μg/g、原儿茶酸35.41~71.54μg/g、绿原酸8.65~28.42μg/g。结论本研究所建立同时测定鼠曲草中3种有机酸类成分的方法简便、快捷、准确,可用于鼠曲草药材的质量控制。

Objective To establish a UPLC-MS/MS method for simultaneous determination of 3 organic acids(caffeic acid,protocatechuic acid and chlorogenic acid)in Gnaphalium affine.Methods The UPLC-MS/MS analysis was performed on a Kinnetex C18(2.1 mm×100 mm,2.6μm)column with acetonitrile-0.1%ammonia as a mobile phase by gradient elution at a flow rate of 0.25 ml/min.The column temperature was set at 40℃.MS detection was performed with multiple reaction monitoring(MRM)mode using negative electrospray ionization.Results Under the chromatographic conditions,the 3 organic acids showed good linear relationship in the linear range(r>0.9984),and the recoveries ranged from 95.00%to 102.55%with the RSD within 2.42%to 3.06%.The con⁃tents of the 3 organic acids in 6 batches of samples were as follows:caffeic acid 10.25-45.12μg/g,protocatechuic acid 35.41-71.54μg/g,and chlorogenic acid 8.65-28.42μg/g.Conclusion The proposed UPLC-MS/MS method for simultaneous determination of the 3 organic acids in G.affine is simple,fast and accurate,which can be used for quality control of G.affine.