HPLC-CAD测定熊去氧胆酸片的含量

Content Determination of Ursodeoxycholic Acid Tablets by HPLC-CAD

目的 建立 HPLC-CAD 法测定熊去氧胆酸片的含量。方法 采用 Sunfire C_(18 )色谱柱(4.6 mm×250 mm,5 μm),流动相为 0.1%甲酸-乙腈-甲醇(32∶58∶10),流速为 1.0 mL·min^(-1),柱温为 35 ℃;CAD 检测器参数:雾化温度 35 ℃,幂率 1.6,采样频率 10 Hz。结果 熊去氧胆酸与相邻的杂质之间分离度良好,在 0.05~1.0 mg·mL^(-1)内线性关系良好(r~2=0.999 7);熊去氧胆酸低、中、高 3 种浓度的平均回收率分别为 99.6%,99.9%,99.9%。3 批样品中熊去氧胆酸的含量测定结果分别为 99.7%,100.3%和 99.8%,与原标准方法相比,结果无明显差异。结论 HPLC-CAD 法操作简单,专属性强,灵敏度高,可以作为熊去氧胆酸片的质量控制和评价方法。

OBJECTIVE To establish an HPLC-CAD method for determination of content of ursodeoxycholic acid tablets.METHODS A Sunfire C_(18 )column(4.6 mm×250 mm,5 μm) was used,the mobile phase was 0.1% formic acid-acetonitrile-methanol(32∶58∶10) and the flow rate was 1.0 mL·min^(-1) with column temperature of 35 ℃.CAD detector parameters:the nebulization temperature was 35 ℃,with power function value of 1.6 and collection frequency of 10 Hz.RESULTS Ursodeoxycholic acid could be well separated with adjacent impurities.The linearity was good in the range of0.05-1.0 mg·mL^(-1)(r~2=0.999 7).The recoveries of ursodeoxycholic acid of the low,medium and high three concentrations were99.6%,99.9% and 99.9%,respectively.The contents of ursodeoxycholic acid in three batches of samples were 99.7%,100.3%and 99.8% respectively,and there was no significant difference compared with the original standard method.CONCLUSION HPLC-CAD method is simple,specific and sensitive,which can be used as the quality control and evaluation method of ursodeoxycholic acid tablets.