顶空气相色谱法检测羟基甲硝唑对照品中的残留溶剂

Determination of Residual Solvents in Hydroxy Metronidazole by Headspace Gas Chromatography

建立羟基甲硝唑中残留溶剂甲醇和丙酮的顶空气相色谱测定方法。采用Agilent-DB624石英毛细管色谱柱(30 m×0.53 mm,1.0μm);以氮气为载气,氢火焰离子化检测器为检测器,进样口温度为200℃,检测器温度为250℃;以起始温度30℃,保持5 min,20℃/min升温至200℃,保持2分钟为程序升温方法;以顶空瓶平衡温度80℃,平衡30 min为顶空条件。结果表明,在该色谱条件下甲醇和丙酮与其他物质分离良好。甲醇在2~360μg/mL范围内线性关系良好,检测线为1.0μg/mL;丙酮在1~600μg/mL范围内线性关系良好,检测限为0.5μg/mL。甲醇回收率为98.0%~102.4%,RSD为0.6%~0.9%;丙酮回收率为97.0%~99.6%,RSD为0.6%~1.0%。本方法操作简单,准确度高,重复性好,可用于羟基甲硝唑中残留溶剂的检测。

A method for the determination of residual solvents in hydroxyl metronidazole was developed by headspace capillary gas chromatography.The two residual solvents were detected by GC with Agilent DB-624 capillary column(30 m×0.53 mm,1.0μm)with FID detector an nitrogen as carrier gas.The temperature of the injection port was maintaining at 200℃and that of detector at 250℃.The column temperature rose by program,and the initial temperature was 30℃and maintained for 5 min.Thereafter the temperature was raised to 200℃at a rate of 20℃/min.Results show that methanol and acetone were finel separated.There were good linearity of methanol in range of 2~360μg/mL,the LOD is1.0μg/mL and acetone in range of 1~600μg/mL,the LOD is 0.5μg/mL.The recovery rate were 98.0%~102.4%(0.6%~0.9%),97.0%~99.6%(0.6%~1.0%),respectively.The method is rapid,accurate,sensitive,and suitable for determination of the residual solvents inhydroxy metronidazole.