HPLC-CAD法测定元胡止痛胶囊中生物碱和香豆素

Determination of alkaloids and coumarins in Yuanhu Zhitong Capsules by HPLC-DAD

目的建立高效液相色谱法联合二极管阵列检测器(HPLC-DAD)法同时测定元胡止痛胶囊中延胡索乙素、盐酸黄连碱、去氢延胡索甲素、延胡索甲素、欧前胡素和异欧前胡素。方法采用HPLC-CAD法,Thermo Hypersil BDS C18色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈–10 mmol/L甲酸铵(甲酸调pH 4.0),梯度洗脱;体积流量0.8 mL/min;CAD雾化器温度为35℃;柱温35℃;进样量为20μL。结果延胡索乙素、盐酸黄连碱、去氢延胡索甲素、延胡索甲素、欧前胡素和异欧前胡素分别在0.041～1.020、0.013～0.320、0.068～1.700、0.041～1.020、0.101～2.520、0.039～0.980μg与峰面积线性关系良好;平均回收率分别为98.41%、98.89%、98.32%、99.35%、98.05%、98.67%,RSD值分别为0.9%、1.4%、0.7%、1.1%、0.7%、0.9%。结论该方法准确、简便、灵敏度高,可用于元胡止痛胶囊中生物碱和香豆素类多成分的质量控制研究。

Objective To establish an HPLC-DAD method for simultaneous determination of tetrahydropalmatine, coptisine hydrochloride, dehydrocorydaline, corydaline, imperatorin, and isoimperatorin in Yuanhu Zhitong Capsules. Methods HPLC-CAD method was adopted on Thermo Hypersil BDS C18 column(250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-10 mmol/L ammonium formate(formic acid tone pH 4.0) with gradient elution. The flow rate was 0.8 m L/min, CAD atomizer temperature was 35℃, temperature of column was set at 35℃, and volume of injection was 20 μL. Results The linear ranges of tetrahydropalmatine, coptisine hydrochloride, dehydrocorydaline, corydaline, imperatorin, and isoimperatorin were 0.041 — 1.020, 0.013 —0.320, 0.068 —1.700, 0.041 —1.020, 0.101 —2.520, and 0.039 —0.980 μg, respectively. The average recoveries were 98.41%, 98.89%, 98.32%, 99.35%, 98.05%, and 98.67%, with RSD of 0.9%, 1.4%, 0.7%, 1.1%, 0.7%, and 0.9%, respectively. Conclusion The method is accurate, simple and sensitive, can be used for the quality control of alkaloids and coumarins in Yuanhu Zhitong Capsules.