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出 处:《分析化学》2010年第4期577-580,共4页Chinese Journal of Analytical Chemistry
基 金:河北省自然基金(No.C2009001069)资助项目
摘 要:利用1-乙基-3-甲基咪唑四氟硼酸盐([Emim][BF4])为顶空溶剂的顶空气相色谱法(HS-GC)快速、准确地分析了药物中的丙酮、四氢呋喃、二氧六环、吡啶及甲苯等有机溶剂残留。采用ZB-1毛细管柱(60m×0.53mm,5.0μm),程序升温方式,顶空瓶平衡温度100℃,平衡时间20min。待测溶剂在所考察的浓度范围内具有良好的线性,平均回收率为90.1%~96.9%;RSD均小于4.2%;检出限分别为0.05,0.07,0.28,0.31及0.04mg/L。室温离子液体作为溶剂使得方法的灵敏度有所提高。The room temperature ionic liquid,1-ethyl-3-methylimidazolium tetrafluoroborate,was used as the alternative solvent and coupled with static headspace gas chromatography to simultaneously determine several residual organic solvents.The analysis was carried out on a ZB-1 capillary column(60 m×0.53 mm,5.0μm)with programmed temperature.The headspace sampler vials was equilibrated at 100℃for 20 min. An excellent separation and good linearity between the response and the concentration range of 3.1-100.0 mg/L,2.3-72.0 mg/L,1.1-36.0 mg/L,0.6-20.0 mg/L and 2.8-89.0 mg/L on acetone,tetrahydrofuran,dioxane,pyridine and toluene respectively were obtained.The average recoveries were 90.1%-96.9%and the RSD was less than 4.2%(n=9).The sensitivity of this method was improved and the detection limits were 0.05,0.07,0.28,0.31 and 0.04 mg/L,respectively.
关 键 词:1-乙基-3-甲基咪唑四氟硼酸盐 顶空气相色谱法 马来酸氯苯那敏 残留溶剂 内标
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