[关键词]
[摘要]
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,5 μm);流动相:80%甲醇-10 mmol/L甲酸铵,梯度洗脱;体积流量:1.0 mL/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:20 μL;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0.51~10.20 μg/mL(r=0.999 4),0.53~10.60μg/mL(r=0.999 3),2.52~50.40μg/mL(r=0.999 5),5.05~101.00μg/mL(r=0.999 4),5.01~100.20μg/mL(r=0.999 8),1.02~20.40μg/mL(r=0.9995)、0.62~12.40 μg/mL(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。
[Key word]
[Abstract]
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, 5 μm) column with 80% methanol - 10 mmol/L ammonium formate as the mobile phase for gradient elution. The flow rate was 1.0 mL/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 20 μL, 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 — 10.20 μg/mL (r = 0.999 4), 0.53 — 10.60 μg/mL (r = 0.999 3), 2.52 — 50.40 μg/mL (r = 0.999 5), 5.05 — 101.00 μg/mL (r = 0.999 4), 5.01 — 100.20 μg/mL (r= 0.999 8), 1.02 — 20.40 μg/mL (r = 0.999 5), and 0.62 — 12.40 μg/mL (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.
[中图分类号]
R286.02
[基金项目]