2-甲氧基雌二醇中有机溶剂残留量的气相色谱法测定

Determination of two residual organic volatile solvents in 2-methoxyestradiol by gas chromatography

目的:测定2-甲氧基雌二醇中残留溶剂甲醇和二氯甲烷的含量。方法:采用气相色谱法检测3批2-甲氧基雌二醇样品中的组分。应用氢火焰离子化检测器(FID),以N,N-二甲基甲酰胺为溶剂,采用HP-INNOWAX柱(30m×0.53mm×1μm),以PEG20M为固定相,柱温45℃,保持3min,然后以20℃/min的速度升温至180℃,保持5min;进样器温度200℃;检测器温度300℃;载气为氮气;分流比为2:1。结果:实现了各组分的基线分离;3批样品中的残留溶剂含量均符合要求。结论:该方法灵敏、准确、可靠,适用于2-甲氧基雌二醇中有机溶剂残留量的测定。

Aim：To establish gas chromatography method to determine the contents of 2 residual organic volatile solvents,methanol and dichloromethane,in 2-methoxyestradiol（2-ME）.Methods：Gas chromatography was employed to determine the contents of residual organic volatile solvents in 2-ME.Sample was dissolved in N,N-dimethylformamide,1μL solution was injected on a HP-INNOWAX silica capillary column,using nitrogen as the carrier gas with split ratio of 2：1.The initial temperature was kept at 45℃for 3 min,then the temperature was raised to 180℃at the rate of 20℃/min,and subsequently sustained for 5 min.The injection port and detector temperatures were 200℃and 300℃,respectively.Results：Under the above conditions,methanol and dichloromethane were separated completely.The contents of two residual organic volatile solvents in the samples were complied with the specification requirements.Conclusion：The method is proved to be accurate,sensitive and reliable.It is suitable to be adopted in the analysis of the tested solvents.