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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 establish a headspace gas chromatographic method for the determination of residues of three kinds of organic solvents such as methanol, ethanol and toluene in azithromycin API. Methods: The analytical column was a DB-624 capillary column (30m × 0.53mm, 3μm). The carrier gas was high purity nitrogen, the flow rate was 1.0ml · min -1, the inlet temperature was 200 ℃ and the column temperature was programmed The temperature was raised to 40 ° C for 2 min and the temperature was raised to 150 ° C at a rate of 15 ° C · min -1 and the temperature was raised to 200 ° C at a rate of 20 ° C min -1 for 8 minutes. FID, detector temperature of 250 ° C, headspace thermostat temperature of 95T, equilibration time of 30 min. Results: The linear ranges of methanol, ethanol and toluene were 6.026 ~ 449.175μg · ml -1, 2.469 ~ 757.650μg · ml -1 and 0.551 ~ 142.200μg · ml -1, respectively. The average recovery Rates were 98.03%, 96.62% and 97.17%, respectively, with RSDs of 0.42%, 0.38% and 0.60%, respectively (n = 9). Conclusion: The method is simple and accurate, the other components do not interfere with the determination, can be used to determine the residues of azithromycin in organic solvents.