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目的:建立清肝疏郁颗粒中胡黄连苷Ⅰ,Ⅱ,芍药内酯苷和芍药苷的HPLC定量分析方法。方法:超声提取目标物;采用HPLC-DAD系统,Diamonsil(2)-C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.05%甲酸水溶液梯度洗脱,检测波长264 nm(胡黄连苷Ⅰ,Ⅱ),230 nm(芍药苷,芍药内酯苷)。结果:胡黄连苷Ⅰ,Ⅱ,芍药苷,芍药内酯苷的线性范围分别为0.067 2~6.72μg(r=0.999 6),0.017 4~17.4μg(r=0.999 8),0.01~10.00μg(r=0.999 5),0.06~6.00μg(r=0.999 1)。加样回收率分别为98.55%,100.95%,97.90%,97.90%;RSD分别为1.7%,2.4%,1.4%,1.7%。结论:该方法准确、灵敏、简便、重复性好,为清肝疏郁颗粒剂的质量控制提供了科学基础。
Objective: To establish a method for the quantitative analysis of picrotoxin Ⅰ, Ⅱ, paeoniflorin and paeoniflorin in “Qinggan Shuyu Granule”. Methods: The target substance was extracted by ultrasonic. The mobile phase was eluted with a gradient of acetonitrile-0.05% formic acid in water by HPLC-DAD system with Diamonsil (2) -C18 column (4.6 mm × 250 mm, Glycosides Ⅰ, Ⅱ), 230 nm (paeoniflorin, paeoniflorin). Results: The linear ranges of picrotoxin Ⅰ, Ⅱ, paeoniflorin and paeoniflorin were 0.067 2 ~ 6.72 μg (r = 0.999 6), 0.017 4 ~ 17.4 μg (r = 0.999 8), 0.01 ~ 10.00 μg r = 0.999 5), and 0.06 to 6.00 μg (r = 0.999 1). The recoveries were 98.55%, 100.95%, 97.90% and 97.90%, respectively. The RSDs were 1.7%, 2.4%, 1.4% and 1.7% respectively. Conclusion: The method is accurate, sensitive, simple and reproducible. It provides a scientific basis for the quality control of Qinggan Shuyu granule.