摘要
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.
出处
《郑州大学学报(医学版)》
CAS
北大核心
2011年第6期915-917,共3页
Journal of Zhengzhou University(Medical Sciences)