顶空气相色谱法测定苯妥英钠中有机溶剂残留量

目的：建立苯妥英钠中甲醇等5种残留溶剂的测定方法.方法：采用顶空毛细管气相色谱法测定,水为溶剂,色谱柱为HP-624（30.0 m × 530 μm,3.00 μm）;载气为氮气;检测器为FID;程序升温,初始温度为40℃,维持5 min,以20℃·min-升温至200℃,保持5 min.结果：测得各残留溶剂的线性关系良好（相关系数＞0.997 2）;平均回收率92.1％～100.9％,检测限为0.5～1.2 μg.结论：该法操作简便,重现性好,结果准确可靠,可用于苯妥英钠中5种残留溶剂的测定.

Determination of Residual Organic Solvents in Phenytoin Sodium by Headspace Gas Chromatography

Objective：To establish a headspace GC method for the determination of residual organic solvents （methanol,ethanol,isopropanol,acetone and chloroform） in phenytoin sodium.Methods：Headspace gas chromatography was adopted using an HP-624 capillary column （30.0 m × 530 μm × 3.00 μm） with nitrogen as the carrier gas and FID as the detector.The initial column temperature was set at 40℃,maintained for 5min,and then raised（20℃ · min-1） to 200℃,and maintained for another 5min.Results：The calibration curves of the five solvents were all linear （r 〉 0.997 2）.The average recoveries were between 92.1% and 100.9%.The detection limits were 0.5-1.2 μg.Conclusion：The method is simple and reproducible with accurate and reliable results,which can be used in the determination of 5 residual organic solvents in phenytoin sodium.