摘要
目的建立气相色谱法测定左氧氟沙星中残留有机溶剂甲醇、乙醇、三氯甲烷和N,N-二甲基甲酰胺。方法以DB-624(30m×0.53mm×3μm)弹性石英毛细管柱为色谱柱,载气为氮气,采用氢火焰离子化检测器,进样口温度为200℃,检测器温度为250℃。顶空进样法测甲醇、乙醇和三氯甲烷,进样量1.0mL;直接进样法测二甲基甲酰胺,进样量1.0μL。这两种方法均采用程序升温。结果甲醇、乙醇、三氯甲烷和N,N-二甲基甲酰胺线性关系r分别为0.999、0.9999、0.9987、0.9988;平均回收率分别为95.9%、92.8%、109.0%、93.2%,RSD分别为2.6%、2.3%、7.1%、7.0%(n=9)。结论本方法灵敏、简单、准确、有效,适用于测定左氧氟沙星中有机溶剂残留。
OBJECTIVE A method for determination of methanol, ethanol, chloroform and DMF in levofloxacin by capillary gas chromatography had been developed. METHODS A DB-624 capillary column （30m × 0.53mm × 3μm） was used with FID detector.The injection port and detector temperatures were 200℃ and 250℃ respectively, nitrogen was used as carrier gas. The contents of methanol,ethanol, chloroform were determined by headspace sampling and the inject volume was 1.0mL.The determination of DMF was carried by directly sampiing and the inject volume was 1.0μL. The two methods used program heating.RESULTS The regression coefficients of methanol,ethanol, chloroform and DMF were 0. 9999,0. 9999,0. 9987and 0. 9988, respectively. The recoveries（n = 9） were 95.9 %, 92.8 %, 109.0 % and 93.2 % respectively with RSD 2.6 %, 2.3 %, 7.1%, 7.0 % accordingly.CONCLUSION The method is sensitive, simple, accurate and efficient, and can be used for the determination of the residual organic volatile solvents in levofloxacin.
出处
《海峡药学》
2008年第3期50-52,共3页
Strait Pharmaceutical Journal
关键词
毛细管气相色谱法
左氧氟沙星
有机溶剂
残留量
Capillary column gas chromatography
Levofloxacin
Organic solvent
Residual volume
