气相色谱法测定磷酸二甲啡烷中有机溶剂残留

目的：采用气相色谱法测定磷酸二甲啡烷原料药中的乙酸乙酯、三氯甲烷和N,N-二甲基甲酰胺（DMF）3种有机溶剂的残留量。方法：采用毛细管气相色谱法,PEG-20M柱,程序升温,以水为溶剂,FID检测器,对乙酸乙酯、三氯甲烷和DMF的残留量进行检测。结果：3种有机溶剂基本实现基线分离且线性关系良好（r均在0.9990以上）,上述3种溶剂残留的检出限范围分别为0.63,0.60和8.92μg·ml-1。3批样品中3种有机溶剂的残留量均符合ICH的规定。结论：该检测方法灵敏、准确、可靠,可用于磷酸二甲啡烷原料的质量控制。

Determination of Residual Organic Solvents in Dimemorfan Phosphate by GC

Objective：To determine the content of chloroform, ethyl acetate and DMF in dimemorfan phosphate by gas chromatog-raphy （GC）. Methods：The capillary gas chromatography was used with a PEG-20M column, programmed temperature, water as the solvent and FID as the detector. Results：The three organic solvents were separated and showed good linear relationship （r〉0. 999 0）. The detection limit of chloroform, ethyl acetate and DMF was 0. 63,0. 60 and 8. 92μg·ml-1 , respectively. The residues of the organ-ic solvents in three batches of the samples all met with the requirements of ICH. Conclusion： The method is sensitive, accurate and reliable, and can be used in the quality control of dimemorfan phosphate.