气相色谱法测定瑞格列奈原料药的有机溶剂残留量

Determination of the residual solvents in repaglinide by GC

目的:建立瑞格列奈原料药残留溶剂的测定方法。方法:采用Agilent DB-FFAP毛细管色谱柱(50 m×0.32mm)、顶空进样法,以FID检测。结果:正己烷、丙酮、乙酸乙酯、乙醇、甲苯分别在7.3～58.4、125.7～1 005.5、125.3～1 002.7、125.9～1 007.2和22.4～179.5μg/ml范围内线性关系良好,平均回收率分别为97.5%、95.6%、96.6%、97.8%和94.8%,RSD分别为1.4%、1.6%、1.7%、1.2%和1.2%。结论:所建立方法专属性好,简便准确,可用于瑞格列奈原料药残留溶剂的限度检查。

Objective：To establish a method for content determination of the residual solvers on repaglinide.Methods： The analysis was performed on a column of Agilent DB-FFAP（50 m×0.32 mm）,used headspace sampling method,detected by FID.Results ：The standard curves of n-hexant,acetone,ethyl acetate,ethanol and toluene were linear within the ranges of 7.3～58.4、125.7～1 005.5、125.3～1 002.7、125.9～1 007.2 and 22.4～179.5 μg/ml,respectively.The average recoveries were 97.5%、95.6%、96.6%、97.8%、94.8%,the RSD were 1.4%、1.6%、1.7%、1.2%、1.2%.Conclusion： The method is specific,simple and accurate for the quality control repaglinide raw materials.,