毛细管气相色谱法测定奥沙利铂原料药中有机溶剂的残留量  

Determination of residual organic solvents in Oxaliplatin by capillary gas chromatography

作　　者：梁然然[1] 吴盛美[1] 訾丽丽[1] 严拯宇[1,2] 

机构地区：[1]中国药科大学分析化学教研室,南京211198 [2]国家药物质量与安全预警教育部重点实验室,南京211198

出　　处：《海峡药学》2013年第4期31-34,共4页Strait Pharmaceutical Journal

摘　　要：目的建立以毛细管气相色谱法检测奥沙利铂原料中2种有机溶剂乙醚、乙醇残留量的方法。方法采用聚乙二醇毛细管柱(30.0m×530μm×3μm);氢火焰离子化检测器(FID);柱温采用程序升温:初温60℃(保持4min),以30℃/min升温至180℃(保持5min);载气为N2;进样口温度:220℃;检测器温度:250℃;丙酮为内标进行测定。结果奥沙利铂原料药中残留溶剂乙醚和乙醇达到完全分离,且均呈现良好的线性关系和回收率,3批样品检测残留溶剂均未超标。结论本测定方法简单、准确,适用于奥沙利铂原料药中残留溶剂的测定。OBJECTIVE To establish a method for the determination of two residual organic solvents（ethanol,diethyl ether） in Oxaliplatin raw material by capillary gas chromatography.METHODS The determination was performed on a polyethylene glycol column（30.0m×530μm×3μm） with FID detection.The initial column temperature was 60℃,maintained it for 4 min,then programmed to 180℃（5min） at the rate of 30℃/min,maintaining it for 5min.N2 was the carrier gas and acetone was the internal standard.The injection port temperature was maintained at 220℃ and the detector temperature was maintained at 250℃.RESULTS Using the established method,two residual organic solvents（ethanol and diethyl ether） in Oxaliplatin raw material were not only separated thoroughly but also behaved good linear relationship and recovery separately.The level of residual organic solvents in three batches of samples analyzed was found totally under quality limit.CONCLUSION The established method is proved simple and accurate,which is suitable for determination of organic solvents in Oxaliplatin.

关 键 词：毛细管气相色谱 乙醚 乙醇 残留溶剂 奥沙利铂 

分 类 号：R927.2[医药卫生—药学]