蒸发光散射检测器-高效液相色谱法测定小儿化毒胶囊中胆酸和猪去氧胆酸含量

Content Determination of Cholic Acid and Hyodeoxycholic Acid in Xiao'er Huadu Capsules by ELSD-HPLC

目的建立同时测定小儿化毒胶囊中胆酸含量和猪去氧胆酸的蒸发光散射检测器-高效液相色谱(ELSD-HPLC)法。方法色谱柱采用Waters Symmetry C_(18)柱(250 mm×4. 6 mm,5μm),流动相为乙腈-0. 1%冰醋酸溶液(40∶60),流速为1 mL/min,柱温为35℃,检测器为ELSD,漂移管温度为98℃,空气流速为3. 0 m L/min。结果胆酸进样量在1. 068～10. 680μg范围内其与峰面积线性关系良好,回归方程为Y=1. 46 X+5. 83(r=0. 999),平均加样回收率为99. 81%,RSD为2. 46%(n=6);猪去氧胆酸进样量在1. 121～11. 210μg范围内其与峰面积线性关系良好,回归方程为Y=1. 46 X+5. 68(r=0. 999),平均加样回收率为101. 40%,RSD为2. 91%(n=6)。结论该方法科学、简便、专属性较强,可有效控制该制剂中人工牛黄的质量。

Objective To establish an ELSD- HPLC method for content determination of cholic acid and hyodeoxycholic acid in Xiao＇er Huadu Capsules. Methods The chromatographic column was Waters Symmetry C18 column（250 mm x4.6 ram, 5 μm）, the mobile phase was acetonitrile -0.1% aceticacid（40： 60）, the flow rate was 1 mL/min, the column temperature was 35 ℃, the detector was ELSD, the temperature of the drift tube was 98 ℃ and the flow rate of the nitrogen gas was 3.0 mL/min. Results Cholic acid showed a good linear relationship within the range of 1. 068- 10. 680 pug, the regression equation was Y= 1.46X＋5.83（ r=0. 999）, the average recovery rate was 99.81% and RSD was 2.46% （n=6）. Hyodeoxycholic acid showed a good linear relationship within the range of 1. 121- 11.210 μg, the regression equation was Y=1.46 X＋5.68（r=0.999）, the average recovery rate was 101.40% and the RSD was 2.91% （ n = 6）. Conclusion The method is scientific, simple and specific, which can efl^ctively control the quality of artificial bezoar in the preparation.