HPLC测定清肝疏郁颗粒剂中4种成分的含量

Determination of Four Components in Qinggan Shuyu Granule by HPLC

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 rapid HPLC-DAD method for the simultaneous determination of four compounds,namely picroside Ⅰ,Ⅱ,paeoniflorin and albiflorin std in Qinggan Shuyu granule. Method： The analytes were extracted by ultrasonic. The separation of the compounds was performed on Diamonsil（2）-C18（ 4. 6 mm × 250 mm,5 μm） column with acetonitrile-0. 05% formic acid solution as mobile phase at the wavelength of 264 nm（ picroside Ⅰ,Ⅱ） and 230 nm（ paeoniflorin,albiflorinstd）. Result： The four analytes demonstrated a good linearity（ r〉0. 999 1） within a relatively wide concentration range（ 0. 067 2-6. 72 μg for picroside Ⅰ,0. 017 4-17. 4 μg for picroside Ⅱ,0. 01-10. 00 μg for paeoniflorin and 0. 06-6. 00 μg for albiflorin std）,and the recoveries ranged between 97. 90%-100. 95%,with RSD of 1. 7%,2. 4%,1. 4%,1. 7%,respectively. Conclusion： The method was found to be accurate,simple and sensitive for the quantitative analysis on the four compounds in Qinggan Shuyu granule.