摘要
目的建立硝酸咪康唑原料残留溶剂的测定方法。方法采用气相色谱法,使用PEG-20M毛细管（30m×0.25mm,0.25μm）色谱柱,柱温采用程序升温,初始温度60℃,保持3min,再以30℃·min^-1升至185℃,保持20min;进样口温度为200℃;检测器为FID;检测器温度为250℃。结果同时测定了硝酸咪康唑原料中的2种有机溶剂,丙酮和甲苯线性范围分别为0.25-1.0mg·mL^-1（r=0.999 8）、0.044 5-0.178mg·mL^-1（r=0.999 6）,平均加样回收率分别为100.3%和99.9%,RSD分别为1.8%和1.3%。结论该方法灵敏、准确,可用于硝酸咪康唑中残留溶剂的检测。
Objective To establish a method for the determination of two residual solvents in miconazole nitrate.Methods The determination was performed on a GB-WAX column（30m×0.25mm,0.25μm）.The column temperature was maintained at 60℃for 3min,and programmed to 185℃at 30℃·min^-1,then held for 20min.FID was used as a detector,and the temperatures of the injector and detector were set at 200and 250℃,respectively.Results Two organic solvents of miconazole nitrate were determined simultaneously in raw materials.The calibration curves were linear in the ranges of 0.25-1.0mg·mL^-1 for acetone（r=0.999 8）,and 0.0445-0.178mg·mL^-1 for toluene（r=0.999 6）.The average recoveries were 100.3%and 99.9%,RSDs were1.8%and 1.3%,respectively.Conclusion The methods were proved to be accurate and sensitive,and can be used for the detection of residual solvents in miconazole nitrate.
出处
《西北药学杂志》
CAS
2014年第4期368-370,共3页
Northwest Pharmaceutical Journal
