HPLC-CAD测定熊去氧胆酸片的含量

Content Determination of Ursodeoxycholic Acid Tablets by HPLC-CAD

关键词:  高效液相色谱-电喷雾检测器  熊去氧胆酸  含量测定  质量控制

Key words:  HPLC-CAD  ursodeoxycholic acid  content determination  quality control

摘要:

目的 建立HPLC-CAD法测定熊去氧胆酸片的含量。方法 采用Sunfire C₁₈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(r²=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。

Abstract:

OBJECTIVE To establish an HPLC-CAD method for determination of content of ursodeoxycholic acid tablets. METHODS A Sunfire C₁₈column(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 of 0.05-1.0 mg·mL^-1(r²=0.999 7). The recoveries of ursodeoxycholic acid of the low, medium and high three concentrations were 99.6%, 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.