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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 method for the simultaneous determination of three organic solvents residues in ursodeoxycholic acid raw material by headspace gas chromatography. Methods: The sample was dissolved in 0.25 mol·L-1 sodium hydroxide solution. The sample was applied on a DB-WAX capillary column (30.0 m × 320 μm × 1.0 μm) using headspace injection-gas chromatography with a FID detector The temperature was raised to 70 ° C for 5 minutes and the temperature was raised to 180 ° C at a rate of 15 ° C · min -1 for 5 minutes. The carrier gas was nitrogen, and the inlet temperature was 200 ° C and the detector temperature was 230 ° C . Results: The tested components could be effectively separated. The linearity of each component in the investigated range was good, r = 0.9976 ~ 0.9996, the average recovery was 91.00% ~ 99.09%. Conclusion: This method can accurately determine the residual amount of acetone, ethanol and N, N-dimethylformamide in UDCA raw material, and has the advantages of simple operation, high accuracy and high sensitivity, and effective control of the quality.