清胰利胆口服液质量标准研究

目的建立清胰利胆口服液中主要活性成分大黄素和大黄酚的RP-HPLC方法,为制订质量标准提供依据。方法采用10（105）均匀试验设计法,优化大黄素、大黄酚的RP-HPLC样品处理;采用9（33）正交试验,优化清胰利胆口服液的生产工艺;采用Agilent 1100 series高效液相色谱仪,Turner ODS色谱柱（4.5×150mm,5 m）;柱温25℃;流速1.0ml.min-1;以乙腈-0.1%冰醋酸溶液为流动相,梯度洗脱;检测波长254nm;进样量20L;结果均匀试验的回归方程为：Y=-320.718＋6.466C＋32.120B（〈0.05）,其最优组合10mL10%的盐酸,85℃水浴40min;正交试验确定最佳生产工艺为20倍量水提取3次,每次10min;大黄素和大黄酚的线性范围分别为14.3~915.2ng（r=0.9996）、20.1~1286.4ng（r=0.9993）;平均加样回收率分别为106.7%和100.1%（n=9）。结论所建立生产工艺稳定,检测方法简便快速,能有效控制清胰利胆口服液的质量。

Study on Quality Standard of Qingyi Lidan oral liquid

Objective To develop a RP-HPLC method for determining the content of emodin and chrysophanol in Qingyi Lidan oral liquid. Methods U10 （ 10^5 ） Uniform design was used to optimize a sample preparation. L9 （33） orthogonal test was employed to optimize the production process of Qingyi Lidan oral liquid. Agilent 1100 series High Performance Liquid Chromatography was used. The column was Turner ODS （4.5×150mm, 5μm）. The mobile phase was composed ofac- etonitrile （A） -0.1% acetic acid （B） solution with gradient elution at a flow rate of 1.0 ml·min^-1, the column temperature was 25℃, and the detect wavelength was 254nm, the injectionvolume was 20L. Results The regression equation of Uniform design was： Y=-320.718＋6.466C＋32.120B （P〈0.05）. The optimum extraction was 20 times as the water, 3 times in extracting and 10 rain each time. The linear ranges ofemodin and chrysophanol were 14.3-915.2ng （r = 0.9996）, 20.1-1286.4ng （r=0.9993）, respectively. Their averagerecoveries （n=9） were 106.7%and 100.1%, respectively. Conclusion The optimum extraction is stable, and the RP-HPLC method is simple, rapid to control the quality of Qingyi Lidan oral liquid.