抗癫痫新药的有机溶剂残留检测

The Determination of Residual Solvents in an Anti-epilepsyDrug by Capillary Gas Chromatography

采用(5%)二苯基-(95%)二甲基硅氧烷毛细管色谱柱(30m×0.25mm×0.25mm),程序升温的色谱条件,分别以溶液直接进样法及顶空进样法,建立毛细管气相色谱法检测抗癫痫新药Q808中有机溶剂的含量,并比较2种不同检测方法。测定了3种有机溶剂残留,分别为甲醇、二氯甲烷、乙酸乙酯。溶液直接进样法能够检测出甲醇和二氯甲烷;顶空进样法3种有机溶剂均可检测,用2种方法检测出的有机溶剂含量均符合要求。通过对2种方法的比较,溶液直接进样法较好。结论显示,Q808中残留的3种有机溶剂含量符合规定,且毛细管气相色谱法的2种方法均可用于Q808中有机溶剂残留的检测,其中溶液直接进样法操作简便、快速,溶液用量少。

（5%） diphenyl-（95%） dimethyl silicone capillary chromatographic column（30m×0.25mm×0.25mm） was used on a programmed column temperature to establish capillary gas chromatography method for detecting the content of the residual solvents in the anti-epilepsy drug（Q808）.The direct injection of solution and the head-space injection were both used to compare the two different methods.Methanol,Methylene chloride and Ethyl Acetate were determined respectively.For the direct injection of solution,methanol and dichloromethane can be detected.For head-space injection,three kinds of organic solvents can be detected,and two methods were selected by meeting the requirements of the organic solvent content.The conclusion showed that the content of three kinds of organic solvent residues in Q808 was in accordance with the provisions.The two methods both can be used to determine the residues of Methanol,Methylene chloride,Ethyl acetate.In which the direct injection of solution is simple,rapid,and with small volume of solution.