HPLC-CAD法测定川芎茶调散中绿原酸、阿魏酸、阿魏酸松柏酯、洋川芎内酯A、Z-藁本内酯、欧前胡素和异欧前胡素

Determination of chlorogenic acid,ferulic acid,coniferly ferulate,senkyunolide A,Z-ligustilide,imperatorin,and isoimperatorin in Chuanxiong Chatiao Powder by HPLC-CAD

目的建立高效液相色谱-电喷雾检测器(HPLC-CAD)法同时测定川芎茶调散中绿原酸、阿魏酸、阿魏酸松柏酯、洋川芎内酯A、Z-藁本内酯、欧前胡素、异欧前胡素。方法采用资生堂Capcell Pak MGⅡC18色谱柱(250 mm×4.6 mm,5μm);流动相:80%甲醇-10 mmol/L甲酸铵,梯度洗脱;体积流量:1.0 m L/min;柱温:40℃;CAD雾化器温度:35℃,采集频率:10 Hz,过滤常数:5.0;进样体积:20μL;稀释剂:70%甲醇。结果绿原酸、阿魏酸、阿魏酸松柏酯、洋川芎内酯A、Z-藁本内酯、欧前胡素、异欧前胡素的质量浓度分别在0.51~10.20μg/m L(r=0.9994),0.53~10.60μg/m L(r=0.9993),2.52~50.40μg/m L(r=0.9995),5.05~101.00μg/m L(r=0.9994),5.01~100.20μg/m L(r=0.9998),1.02~20.40μg/m L(r=0.9995)、0.62~12.40μg/m L(r=0.9993)线性关系良好;平均回收率分别为99.46%、98.65%、98.48%、98.74%、98.60%、98.69%、98.58%,RSD值分别为1.62%、0.87%、1.03%、1.20%、1.25%、0.69%、0.66%。结论方法准确、重复性好,为川芎茶调散的质量研究提供了更加全面的方法。

Objective To develop an HPLC-CAD method for simultaneous determination of chlorogenic acid,ferulic acid,coniferly ferulate,senkyunolide A,Z-ligustilide,imperatorin,and isoimperatorin in Chuanxiong Chatiao Powder.Methods Chromatographic separation was performed on a Capcell Pak MGⅡC18(250 mm×4.6 mm,5μm)column with 80%methanol-10 mmol/L ammonium formate as the mobile phase for gradient elution.The flow rate was 1.0 m L/min,and the column temperature was maintained at 40℃.The nebulization temperature of detector was 35℃,the acquisition frequency was 10 Hz,and the filtration constant was 5.0.Injection volume was 20μL,and diluent was used as 70%methanol.Results Chlorogenic acid,ferulic acid,coniferly ferulate,senkyunolide A,Z-ligustilide,imperatorin,and isoimperatorin had good linear in the ranges of 0.51—10.20μg/m L(r=0.9994),0.53—10.60μg/m L(r=0.9993),2.52—50.40μg/m L(r=0.9995),5.05—101.00μg/m L(r=0.9994),5.01—100.20μg/m L(r=0.9998),1.02—20.40μg/m L(r=0.9995),and 0.62—12.40μg/m L(r=0.9993),respectively.The average recoveries were 99.46%,98.65%,98.48%,98.74%,98.60%,98.69%,and 98.58%with RSD values of 1.62%,0.87%,1.03%,1.20%,1.25%,0.69%,and 0.66%,respectively.Conclusion The method is accurate and reproducible to provide a more comprehensive method for the quality control of Chuanxiong Chatiao Powder.