前列倍喜片中槲皮素和山奈素HPLC检测方法的建立及其评价

Establishment and evaluation of method of HPLC for determination of quercetin and kaempferol in Qianliebeixi tablet

目的:建立前列倍喜片中槲皮素和山奈素含量的高效液相色谱(HPLC)法测定方法,为工业生产的质量控制提供依据。方法:采用HPLC测定前列倍喜片中槲皮素和山奈素的含量,检测条件:Shimpack VP-ODSC18(150.0mm×4.6mm,5μm)色谱柱,流动相为乙腈-0.2%磷酸溶液(30∶70),检测波长为370nm,柱温为30℃。结果:槲皮素在0.042 6～0.639 0μg范围内有良好线性关系,回归方程为Y=-10 931+1 426 905X,r=0.999 8,平均回收率98.5%,RSD为2.61%(n=6);山奈素在0.045 4～0.726 4μg范围内有良好线性关系,回归方程为Y=-558 68+1 656 625X,r=0.999 2,平均回收率100.3%,RSD为2.28%(n=6);以精密度实验、稳定性实验和重复性实验考察的RSD分别为1.66%、2.11%和1.35%。经测试并结合生产实际情况限定前列倍喜片中槲皮素和山奈素的含量不少于0.7mg/粒。结论:HPLC测定前列倍喜片中槲皮素和山奈素含量的方法准确、简单可行,重复性好,为控制前列倍喜片的质量提供了科学依据。

Objective To establish the method of high performance liquid chromatography（HPLC） for determining quercetin and kaempferol in Qianliebeixi tablet,and provide basis for the quality control of industrial production.Methods The method of HPLC was developed to determine quercetin and kaempferol in Qianliebeixi tablet.The developed conditions of HPLC were as follows：the shim-pack VP-ODS C18（150.0 mm×4.6 mm,5 μm）,Acetonitrile-0.2% phosphoric acid solution（30∶70） mobile phase,370 nm detection wave length,and 30℃ column temperature.Results The linear range of quercetin was 0.042 6-0.639 0 μg,the regression equation was Y=-10 931＋1 426 905X,r=0.999 8,the average recovery was 98.5%,and the RSD was 2.61%（n=6）.The linear range of kaempferol was 0.045 4~0.726 4 μg,the regression equation was Y=-55 868＋1 656 625X,r=0.999 2,the average recovery was 100.3%,and the RSD was 2.28%（n=6）.The RSD in accuracy,stability and repeatability test were 1.66%,2.11%,and 1.35%,respectively.The content of quercetin or kaempferol in Qianliebeixi tablet was limited not less than 0.7 mg per one tablet under the developed condition.Conclusion The method of HPLC for determining quercetin and kaempferol in Qianliebeixi tablet is accurate,simple and reliable,which provides the basis for the quality control of Qianliebeixi tablet.