顶空气相色谱法测定熊去氧胆酸中3种有机溶剂残留量

Determination of Three Residual Solvents in Ursodeoxycholic Acid by Headspace Gas Chromatography

目的：建立顶空气相色谱法同时测定熊去氧胆酸原料药中3种有机溶剂残留量的方法。方法：用0.25 mol·L^-1的氢氧化钠溶液溶解样品,采用顶空进样-气相色谱法,应用FID检测器,在DB-WAX毛细管色谱柱（30.0 m×320μm×1.0μm）上程序升温（起始温度70℃,保持5分钟,再以15℃·min^-1的升温速率升至180℃,保持5分钟）,载气为氮气,进样口温度200℃,检测器温度230℃。结果：待测组分均能得到有效分离,各组分在所考察的浓度范围内线性关系良好,r=0.9976-0.9996,平均回收率为91.00%-99.09%。结论：本方法可准确测定熊去氧胆酸原料药中丙酮、乙醇及N,N-二甲基甲酰胺的残留量,操作简便、准确度和灵敏度高,可达到有效控制其质量的目的。

Objective： To establish a headspace gas chromatography method for the determination of three residual solvents in ursodeoxycholic acid. Methods： Samples were resolved by 0.25 mol·L^-1Na OH, and then the concentration of residual solvents were measured by headspace gas chromatography using FID detector and DB-Wax capillary column（30.0 m×320 μm×0.5 μm） with temperature program（the initial temperature was kept at 70 ℃ for 5 min, then the temperature was raised to 180 ℃ at the rate of 15 ℃·min^-1and kept for 5 min）. The inlet temperature was controlled at 200 ℃, and the detector temperature was 230 ℃, with nitrogen as the carrier gas.Results： The linear range（r=0.9976-0.9996） were satisfactory and three residual solvents were completely separated. The average recovery rates were 91.00%-99.09%. Conclusion： This method is simple, accurate and sensitive for detection of three residual solvents（acetone, ethyl alcohol and N, N-dimethylformamide） in ursodeoxycholic acid, and can be used for quality control.