复方小叶枇杷片水煎液中总黄酮和黄芩苷含量测定

Determination of the Contents of Total Flavone and Baicalin in Decoction of Compound Xiaoyepipa Tablets

目的 :建立复方小叶枇杷片水煎液中总黄酮和黄芩苷的含量测定方法 ,为制剂质量控制提供依据。方法 :紫外分光光度(UV)法测定总黄酮含量 ;反相高效液相色谱 (RP -HPLC)法测定黄芩苷含量 ,采用ZORBAXSB -C18 色谱柱 ,流动相为乙腈 -水 (27∶75) ,流速为0 7ml/min ,检测波长为280nm ,柱温为室温 ,外标法计算含量。结果 :UV法测定总黄酮在8 09～48 53μg/ml浓度范围内线性关系良好 (r=0 9999) ,平均加样回收率分别为100 33 %、99 79 %、99 85 % ,标准差分别为1 53 %、1 27 %、1 76 % (n=5)。RP -HPLC法测定黄芩苷在3 84～57 60μg/ml浓度范围内线性关系良好 (r=0 9998) ,平均回收率分别为100 93 %、99 07 %、100 90 % ,标准差分别为1 50 %、2 22 %、1 09 % (n=5)。结论 :本方法测定结果准确、可靠 ,重现性好 ,能满足制剂中间体质量控制的要求。总黄酮测定中反应时间和测定时间对测定结果影响较大 。

OBJECTIVE:To determine the contents of total flavone and baicalin in decoction of compound Xiaoyepipa tablets so as to provide a basis for quality control of the preparation.METHODS:The quantitative determination of total flavone was performed with UV-spectrophotometry and that of baicalin with RP-HPLC.The RP-HPLC conditions were:Zorbax SB-C 18 column(4.6mm×15cm,5μm)at room temperature;flow rate,0.7ml/min;detected wavelength,280nm;acetonitrile-water(25∶75)adjusted pH to2.7by H 3 PO 4 as mobile phase.The content of baicalin was calculated by external standard method.RESULTS:A linearity was obtained from8.09μg/ml to48.53μg/ml of total flavone with a good correlation(r=0.9999,n=6).The average recoveries and relative standard deviations(RSD)of to talflavon were 100.33%,99.79%,99.85%and1.53%,1.27%,1.76%(n=5)respectively.A linearity was obtained from3.84μg/ml to57.60μg/ml of baicalin with a good correlation(r=0.9998,n=7).The average recoveries and relative standard deviations(RSD)of baicalin were100.93%,99.07%,100.90%,and1.50%,2.22%,1.09%(n=5)respectively.CONCLUSION:This method is accurate,reliable and reˉpeatable and can meet the demands of quality control for midbodies of the preparation.In determination of total flavone,the duration of reaction and time of determination should be strictly controlled becasuse of their obvious influence on the results obtained.