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室温离子液体作为静态顶空气相色谱法测定药物中残留溶剂的基质介质。

Room temperature ionic liquid as matrix medium for the determination of residual solvents in pharmaceuticals by static headspace gas chromatography.

作者信息

Liu Feng-Hua, Jiang Ye

机构信息

Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang City, China.

出版信息

J Chromatogr A. 2007 Oct 5;1167(1):116-9. doi: 10.1016/j.chroma.2007.08.034. Epub 2007 Aug 17.

Abstract

Using new solvent room temperature ionic liquid (IL) matrix media, testing of residual solvents in pharmaceutical preparations with static headspace gas chromatographic (SH-GC), is described. The purpose of this work was to demonstrate the feasibility of IL as diluent, six solvents utilized in synthesis of Adefovir Dipivoxil: acetonitrile, dichloromethane, N-methyl-2-pyrrolidone (NMP), toluene, dimethylformamide (DMF), n-butyl ether were dissolved in IL: 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim]BF(4)). The method of external standard was used for quantitative analysis. Its performance was evaluated and validated: all the RSD were lower than 10%, the limits of detection were all of the ppm level and the method was both accurate and linear. And better sensitivities for the six solvents were gained with [bmim]BF(4) as diluent comparing with DMSO.

摘要

本文描述了使用新型溶剂室温离子液体(IL)基质介质,采用静态顶空气相色谱法(SH-GC)检测药物制剂中的残留溶剂。这项工作的目的是证明IL作为稀释剂的可行性,将阿德福韦酯合成中使用的六种溶剂:乙腈、二氯甲烷、N-甲基-2-吡咯烷酮(NMP)、甲苯、二甲基甲酰胺(DMF)、正丁醚溶解在IL:1-丁基-3-甲基咪唑四氟硼酸盐([bmim]BF(4))中。采用外标法进行定量分析。对其性能进行了评估和验证:所有相对标准偏差(RSD)均低于10%,检测限均为ppm级别,该方法准确且线性良好。与二甲基亚砜(DMSO)相比,以[bmim]BF(4)作为稀释剂时,对这六种溶剂具有更高的灵敏度。

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