顶空气相色谱法检测羟基甲硝唑中的残留溶剂

Determination of Residual Solvents in Hydroxy by Headspace Gas Chromatography

关键词:  羟基甲硝唑  顶空气相色谱法  残留溶剂

Key words:  Hydroxy metronidazole  Headspace gas chromatography  Residual solvents

摘要:

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,1.0 μm)；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2~360 μg/mL范围内线性关系良好,检测线为1.0 μg/mL；丙酮在1~600 μg/mL范围内线性关系良好,检测限为0.5 μg/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。

Abstract:

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, 1.0 μm)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 2~360 μg/mL , the LOD is1.0μg/mL and acetone in range of 1~600μg/mL, the LOD is 0.5 μg/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.