目的 建立高效液相色谱–电雾式检测器（HPLC-CAD）法测定人工牛黄甲硝唑胶囊中胆酸、去氧胆酸、鹅去氧胆酸和猪去氧胆酸。方法 采用Waters SunFire C₁₈色谱柱（250 mm×4.6 mm，5 μm）；流动相为乙腈–0.1%甲酸溶液，进行梯度洗脱；体积流量为1.0 mL/min；柱温35 ℃；进样量20 μL；电雾式检测器，雾化温度：35 ℃；幂率：1.0；采样频率：10 Hz；过滤常数：10 s。结果 胆酸、去氧胆酸、鹅去氧胆酸和去氧胆酸在一定质量浓度范围内线性关系良好，其平均回收率分别为102.1%、101.5%、100.9%、101.6%，RSD值分别为1.40%、1.87%、1.34%、1.69%。结论 本法操作简单，灵敏度高，重现性好，可用于人工牛黄甲硝唑胶囊的质量控制。

Objective To establish a high performance liquid chromatography-charge aerosol detector (HPLC-CAD) method for the determination of cholic acid, deoxycholic acid, chenodeoxycholic acid, and hyodeoxycholic acid in Galculus Bovis and Metronidazole Capsules. Methods A Waters SunFire C₁₈ column (250 mm × 4.6mm, 5 μm) was used in gradient elution with the mobile phase acetonitrile-0.1% formic acid. The volumetric flow rate was 1.0 mL/min, column temperature was 35 ℃, and injection volume was 20 μL. The detector of CAD was applied with nebulization temperature at 35 ℃, power function value (PFV) at 1.0, collection frequency at 10 Hz, and filter constant at 10 s. Results Cholic acid, deoxycholic acid, chenodeoxycholic acid, and hyodeoxycholic acid had good linear relationships within a certain concentration range, with average recovery rates of 102.1%, 101.5%, 100.9%, and 101.6%, respectively, and with RSD values of 1.40%, 1.87%, 1.34%, and 1.69%, respectively. Conclusion The method is simple, sensitivity, and reproducible, which is suitable for the quality control for Galculus Bovis and Metronidazole Capsules.

R927.2

江苏省药品监督管理局科研计划项目（202377）；泰州市科技支撑计划社会发展（指导性）项目（46）