Liu Feng-Hua, Jiang Ye
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang City, China.
J Chromatogr A. 2007 Oct 5;1167(1):116-9. doi: 10.1016/j.chroma.2007.08.034. Epub 2007 Aug 17.
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.
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。