两种方法测定熊去氧胆酸含量的研究

Comparison of two methods for the determination of Ursodeoxycholic acid

采用高效液相色谱法和酸碱滴定法对熊去氧胆酸进行含量测定。以DiamonsilTMC18柱为色谱柱,采用乙腈∶0.001 mol/L磷酸二氢钾溶液(50∶50,用磷酸调节pH值至2.0)为流动相,流速1.0 mL/min,检测波长为205 nm;采用氢氧化钠液(0.1 mol/L)为滴定液,中性乙醇为溶剂,酚酞为指示液,进行酸碱滴定。两种方法测定结果基本一致。用高效液相色谱法熊去氧胆酸在0.075 4～2.262 mg/mL与峰面积呈良好的线性关系(r=0.999 7,n=6),平均回收率为99.2%,RSD=0.5%;酸碱滴定法重现性良好,RSD=0.23%。采用高效液相色谱法专属性强、准确;采用酸碱滴定操作简便、准确、重现性好。

To determine the content of Ursodeoxycholic acid by HPLC and acid-base titration.HPLC was performed on DiamonsilTM C18.The mobile phase was acetonitrile ∶ 0.001 mol/L sodium dihydrogen phosphate solution（50 ∶ 50,adjust pH 2.0 with H2PO4）at a flow rate of 1.0 mL/min,the detective wavelength was 205 nm;Using sodium hydroxide titration solution（0.1 mol/L）as the titrant,neutral alcohol as solvent,phenolphthalein indicator solution for acid-base titration.The results of the two methods showed no difference.The good linear relationship was 0.075 4～2.262 mg/mL（r=0.999 7,n=6）and the average recovery was 99.2% and RSD was 0.5% by HPLC.Acid-base titration method was good reproducibility and RSD was 0.23%.HPLC is specific,accurate;acid-base titration is simple,feasible and reproducible.