LC-MS/MS法测定复方益母草膏中有效成分的含量

Determination of active ingredients in Fufang Yimucao Gao by LC- MS / MS

目的建立高效液相色谱-四级杆串联质谱法(LC-MS/MS)测定复方益母草膏中水苏碱和益母草碱的含量。方法样品以甲醇超声提取后,采用色谱柱为Agilent ZORBAX C18(150 mm×4.6 mm,5μm),流动相为甲醇-体积分数为0.1%的甲酸溶液(体积比为80∶20),质谱采用ESI源正离子-MRM模式下检测,流速为0.4 m L·min^(-1)。结果水苏碱的线性为14.0~140μg·L^(-1),益母草碱的线性为1.50~15.0μg·L^(-1),回收率均在92.1%~100.7%。结论 LC-MS/MS法适用于测定复方益母草膏中水苏碱和益母草碱的含量,同时为控制复方益母草膏的质量提供了依据。

Objective To develop an HPLC-MS / MS method for determination of stachydrine and leonurine in Fufang Yimucao Gao. Methods The chromatographic separation was achieved on a Agilent ZORBAX C18（150 mm × 4. 6 mm,5 μm）column with a mobile phase of methyl alcohol- 0. 1%（φ）formic acid in water（V∶ V = 80∶20）. The flowrate was 0. 4 m L·min^-1. Results The calibration curve was linear within the range of 14. 0-（-1）40 μg·L^-1or stachydrine and 1. 50-（-1）5. 0 μg·L^-1or leonurine,respectively. The recoveries were from 92. 1% to 100. 7%. Conclusions The method was suitable for determination of stachydrine and leonurine. It can be used for the quality control of Fufang Yimucao Gao.