新药磺胺嘧啶锌中有机溶剂残留量测定

Determination of Residual Organic Solvents in New Drug Sulfadiazine Zinc

建立了国家二类新药磺胺嘧啶锌中有机溶剂甲醇和丙酮残留量的毛细管顶空气相色谱分析法。采用PEG-20M弹性石英毛细管色谱柱,F ID检测器,程序升温方法,以氮气为载气。两种有机溶剂完全分离,在浓度范围内具有良好的线性(r均大于0.999),丙酮和甲醇的检出限分别为3.7m g/L和2.9m g/L,精密度RSD均小于1%,平均回收率分别为101.1%和100.8%.经实验方法学验证,该方法灵敏、准确可靠,适用于磺胺嘧啶锌原料药中有机溶剂残留量的测定。

A method for determination of residual organic solvents,acetone and methyl alcohol,in second grade national new medicine sulfadiazine zinc was established by capillary headspace gas chromatograpy.A PEG-20M elasticity quartz capillary column was used with procedural column temperature control.The detector was FID with nitrogen as carrier gas.The calibration curves of two solvents were linear in concentration range（r0.999）.The average recoveries of acetone and methyl alcohol were 101.1% and 100.8%,respectively.The detection limits were 3.7mg/L and 2.9mg/L,respectively.RSD was both less 1%.The method is simple,accurate and sensitive with good reproducibility,that can be used for the determination of the residual organic solvents in sulfadiazine zinc.