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目的建立气相色谱法分离并测定阿奇霉素原料药中甲醇、乙醇、丙酮、乙酸乙酯、二氯甲烷、氯仿6种残留溶剂的含量。方法以OV-1701弹性石英毛细管柱为色谱柱(30 m×0.32 mm,0.5μm),载气为氮气,采用氢火焰离子化检测器,进样口温度为200℃,检测器温度为240℃,柱温采用程序升温(30℃、保持4 min,以25℃.min-1升至120℃、保持5 min),以二甲亚砜为溶剂,进样量1μL。结果甲醇、乙醇、丙酮、乙酸乙酯、二氯甲烷、氯仿在各自的浓度范围内,其峰面积与内标的峰面积比值与浓度呈良好的线性关系,r为0.999 1~0.999 6,平均加样回收率为94.9%~99.6%(n=9)。结论该法分离完全,操作简便快速,灵敏度高,精密度良好,是一种较好的测定原料药中残留溶剂含量的方法。
Objective To establish a gas chromatographic separation and determination of azithromycin APIs methanol, ethanol, acetone, ethyl acetate, methylene chloride, chloroform 6 kinds of residual solvent content. Methods The OV-1701 elastic silica capillary column (30 m × 0.32 mm, 0.5 μm) was used. The carrier gas was nitrogen and the flame ionization detector was used. The inlet temperature was 200 ℃ and the detector temperature was 240 ℃ . The temperature of the column was raised by programmed temperature (30 ℃, kept for 4 min, raised to 120 ℃ at 25 ℃ .min-1 for 5 min), and the sample volume was 1μL with dimethyl sulfoxide. Results The ratios of peak areas to internal standard peak areas of methanol, ethanol, acetone, ethyl acetate, methylene chloride and chloroform showed a good linear relationship with the concentration in the range of their respective concentrations, with r ranging from 0.999 1 to 0.999 6, The average recoveries ranged from 94.9% to 99.6% (n = 9). Conclusion The method is complete separation, simple and rapid operation, high sensitivity, good precision, is a better method for the determination of residual solvents in APIs.