气相色谱法测定阿奇霉素原料药中残留的6种有机溶剂的含量

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。

Determination of the contents of six kinds of organic solvent residue in azithromycin drug by GC

Objective To establish an GC method for determination of the residual amount of six kinds of organic solvents (methanol, ethanol, acetone，ethyl acetate, dichloromethane, trichloromethane) in azithromycin crude drug. Methods A column of OV-1701( 30 m× 0.32 mm, 0.5 μm) was used with FID as detector, the nitrogen was selected as carrier gas. The injector temperature was 200 ℃, the detector temperature was 240 ℃, and the column temperature was programmed raised: 30℃, 4 min; 25 ℃·min^-1 was raised to 120 ℃; 120 ℃, 5 min)]. The solvent was dimethyl sulfoxide, the sample size was 1 μL. Results The pick area ratio of methanol, ethanol, acetone, ethyl acetate, dichloromethane, trichloromethane to internal standard and concentration showed good linearity(r=0.999 1-0.999 6). The average recoveries (n=9) were in the range of 94.9%-99.6%（n=9）. Conclusions The method can separate the solvents completely. It is simple, rapid, sensitive and precise. It’s a good method for the determination of the organic solvent residues in the drug.