顶空气相色谱法测定米非司酮中的5种残留溶剂

目的建立顶空气相色谱法分析米非司酮中甲醇、二氯甲烷、乙酸乙酯、四氢呋喃、吡啶5种溶剂残留量的测定方法。方法采用Agilent DB-624弹性石英毛细管柱（30m×0.53mm×3μm）作为分析用色谱柱,以氮气为载气,FID检测器,以二甲亚砜为溶剂,顶空瓶平衡温度为90℃,平衡时间为30min。结果5种溶剂在各自的浓度范围内具有良好的线性关系,相关系数均为0.999以上,平均回收率分别为98.7%、96.9%、95.7%、95.1%和95.2%,最低检测限分别为0.000578%、0.0002588%、0.000745%、0.000211%和0.001196%。结论本方法简单,结果准确,重复性好,灵敏度高,适用于米非司酮中5种残留溶剂的测定。

Determination of 5 Kinds of Residual Solvents in Mifepristone by Using Headspace Gas Chromatography

OBJECTIVE To establish a headspace gas chromatography method for determination of five residual solvents including ethanl, dichloromethane, ethyl acetate, tetrahydrofuran and pyridininrn in mifepristone. METHODS The determination was performed on an Agilent DB-624 Capillary column（30 m×0.53 mm×3 μm） with nitrogen as carrier gas and FID as detector. Dimethyl sulfoxide was used as solvent, and the equilibrium temperature and time of headspace vial was 90 ℃ and 30 min, respectively. RESULTS Five residual solvents showed good linearity（r〉0.999） in the concentration ranges, respectively. The average recovery were 98.7%, 96.9%, 95.7%, 95.1% and 95.2%, respectively, and the LOD were 0.000 578%, 0.000 258 8%, 0.000 745%, 0.000211%, 0.001 196 %, respectively. CONCLUSION The method is simple, accurate, repeatable and sensitive. It is suitable for the determination of residual solvents in mifepristone.