摘要
目的:建立HPLC-ELSD法同时测定参芪颗粒中党参炔苷、芒柄花素、黄芪皂苷Ⅰ、黄芪皂苷Ⅱ、黄芪皂苷Ⅲ和黄芪甲苷(黄芪皂苷Ⅳ)的含量测定方法。方法:采用Agilent C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.5%(v/v)醋酸水溶液为流动相,进行梯度洗脱,流速1.0 m L·min^(-1),柱温35℃;使用蒸发光散射检测器,载气气压为2.76×(10)~5 Pa,漂移管温度为70℃。结果:在34 min内,参芪颗粒中6个成分(党参炔苷、芒柄花素、黄芪皂苷Ⅰ、黄芪皂苷Ⅱ、黄芪皂苷Ⅲ和黄芪甲苷)完全分离,峰面积的对数与进样量的对数呈良好的线性关系(r=0.999 5~0.999 9);平均回收率分别为96.7%、99.5%、99.5%、98.7%、99.6%、97.4%。3批样品中党参炔苷、芒柄花素、黄芪皂苷Ⅰ、黄芪皂苷Ⅱ、黄芪皂苷Ⅲ和黄芪甲苷含量分别在0.10~0.13、0.008 6~0.012 1、0.014~0.018、0.056~0.060、0.002 3~0.004 1、0.055~0.066 mg·g-1。结论:该方法经方法学验证可用于参芪颗粒的质量控制。
Objective： To establish an HPLC-ELSD method for simultaneous determination of lobetyolin, formononetin and astragalosides ⅠⅡⅢ Ⅳ in Shenqi granules. Methods： The separation was performed on an Agilent C18 column （ 250 mm × 4.6 mm, 5μm ） with gradient elution at a temperature of 35℃. The aeetonitrile and 0.5% （ v/v ） acetic acid was used as the mobile phase with a flow rate of 1.0 mL· min^-1 . The detector was ELSD, of which the drift tube temperature was maintained at 70 ℃ and the pressure of nebulizing gas was 2.76 × 10^5 Pa. Results： The six compounds （ lobetyolin,formononetin and astragalosides ⅠⅡⅢ Ⅳ ） were completely separated within 34 rain. The regression equation showed good liner relationship between logarithm of the peak area and logarithm of the content of each compound （ r=0.999 5-0.999 9 ）. The average recoveries were 96.7%, 99.5%, 99.5%, 98.7%, 99.6%, and 97.4%, respectively. The contents of lobetyolin, formononetin and astragalosides ⅠⅡⅢ Ⅳ in 3 samples were 0.10-0.13,0.008 6-0.012 1,0.014-0.018, 0.056-0.060, 0.002 3-0.004 1 and 0.055-0.066 mg·g^-1, respectively. Conclusion： The established method is validated by methodology, and is suitable for the quality control of Shenqi granules.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2016年第1期68-73,共6页
Chinese Journal of Pharmaceutical Analysis
基金
国家科技重大专项课题(2014ZX09304307-2)
