毛细管气相色谱法测定溴甲基纳曲酮中有机溶剂-中国现代应用药学.PDFVIP

·药物分析与检验 · 毛细管气相色谱法测定溴甲基纳曲酮中有机溶剂残留量 滕菁菁，李清，姬巍，毕开顺*(沈阳药科大学药学院，沈阳 110016) 摘要：目的 建立以毛细管气相色谱法测定溴甲基纳曲酮中二氯甲烷、丙酮、甲醇、甲基叔丁基醚、乙酸乙酯和甲苯 6 种有机溶剂残留量的方法。方法 采用DB-WAX(30.0 m×0.25 mm ，0.25 μm)毛细管柱，氢火焰离子化检测器(FID) ，载气 1 ，进样口温度为240 ℃，检测器温度为250 ℃，柱温为程序升温。结果 甲基叔丁基醚、 为氮气，柱流量为1.0 mL·min 丙酮、乙酸乙酯、甲醇、二氯甲烷和甲苯6 种有机溶剂均得到有效分离，回收率及线性关系皆良好，且 3 批样品中有机 溶剂残留量均符合规定。结论 该方法操作简便，精密度好，准确可靠，可用于溴甲基纳曲酮中有机溶剂残留量的测定。 关键词：溴甲基纳曲酮；毛细管气相色谱法；有机溶剂残留量 中图分类号：R917.101 文献标志码：A 文章编号：1007-7693(2012)02-0153-04 Determination of Residual Organic Solvents in Naltrexone Methylbromide by Capillary Gas Chromatography * TENG Jingjing, LI Qing, JI Wei, BI Kaishun (School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China) ABSTRACT: OBJECTIVE To establish a capillary GC method for the determination of residual organic solvents including methylene chloride, acetone, methanol, methyl tert-butyl ether, ethyl acetate and toluene in naltrexone methylbromide. METHODS The residual organic solvents were separated on DB-WAX capillary column (30.0 m×0.25 mm, 0.25 μm). FID was used as detector with a temperature of 250 ℃, and the inlet temperature was 240 ℃ . The carrier gas was nitrogen, and the flow rate was 1.0 mL·min1. Column temperature was programmed set. RESULTS The six residual organic solvents consisting of methyl tert-butyl ether, acetone, ethyl acetate, methanol, methylene chloride and toluene were completely separated, the recovery rate and linear relationship were good, and three batches of samples coincided with the requirements. CONCLUSION The method is simple, accurate, sensitive and reproducible, it can be used for the determination of the residual organic solvents in naltrexone methylbromide. KEY WORDS: naltrexone meth