顶空气相色谱法测定阿奇霉素中的有机溶剂残留量

Determination of Residual Organic Solvents in Azithromycin by HS-GC

目的:建立测定阿奇霉素原料药申甲醇、乙醇、甲苯等3种有机溶剂残留量的顶空气相色谱法。方法:分析柱为DB-624毛细管柱(30m×0.53mm,3μm),载气为高纯氮气,流速为1.0ml·min^(-1),进样口温度为200℃,柱温为程序升温,初始温度为40℃,保持2min,以15℃·min^(-1)的速度升温至150℃,再以20℃·min^(-1)的速度升温至200℃保持8min,检测器为FID,检测器温度为250℃,顶空恒溫箱温度为95T,平衡时间为30min。结果:甲醇、乙醇、甲苯的线性范围分别为6.026~449.175μg·ml^(-1),2.469~757.650μg·ml^(-1),0.551~142.200μg·ml^(-1),平均回收率分别为98.03%,96.62%,97.17%,RSD分别0.42%,0.38%,0.60%(n=9)。结论:该法简便,准确,其他组分不干扰测定,可用于测定阿奇霉素中的有机溶剂残留量。

Objective： To established an HS-GC method to determine the content of residual organic solvents in azithromycin. Method： A DB-624 column （30 m ×0.53 mm, 3 μm） was used. The carrier gas was high purity nitrogen. The flow rate was 1.0 ml · min-1. The injector temperature was 200℃. The column temperature was programmed raised. The initial temperature was 40℃, kept 2min, then raised the temperature to 150℃ with the rate of 15℃ per minute, then raised the temperature to 200% with the rate of 20℃ per minute and kept 8 rain. The FID detector was used and the temperature was 250~C. The headspace vials equilibrium tem- perature was 95℃ and the balance time was 30 min. Result： The linear range of methanol, ethanol and toluene was 6.026-449. 175, 2.469-757. 650 and 0. 551-142. 200 μg · ml ^-1 , respectively. The average recovery was 98.03% , 96.62% and 97.17% with RSD of 0.42%, 0.38 % and 0.60% （n = 9）, respectively. Conclusion： The method is convenient and accurate without any interference, and can be used for the determination of residual organic solvents in azithromycin.