目的 建立高效液相色譜–電霧式檢測器（HPLC-CAD）法測定人工牛黃甲硝唑膠囊中膽酸、去氧膽酸、鵝去氧膽酸和豬去氧膽酸。方法 采用Waters SunFire C₁₈色譜柱（250 mm×4.6 mm，5 μm）；流動相為乙腈–0.1%甲酸溶液，進(jìn)行梯度洗脫；體積流量為1.0 mL/min；柱溫35 ℃；進(jìn)樣量20 μL；電霧式檢測器，霧化溫度：35 ℃；冪率：1.0；采樣頻率：10 Hz；過濾常數(shù)：10 s。結(jié)果 膽酸、去氧膽酸、鵝去氧膽酸和去氧膽酸在一定質(zhì)量濃度范圍內(nèi)線性關(guān)系良好，其平均回收率分別為102.1%、101.5%、100.9%、101.6%，RSD值分別為1.40%、1.87%、1.34%、1.69%。結(jié)論 本法操作簡單，靈敏度高，重現(xiàn)性好，可用于人工牛黃甲硝唑膠囊的質(zhì)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

江蘇省藥品監(jiān)督管理局科研計(jì)劃項(xiàng)目（202377）；泰州市科技支撐計(jì)劃社會發(fā)展（指導(dǎo)性）項(xiàng)目（46）